# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Leigh Anna M. Steele' _publ_contact_author_email lsteele@sandia.gov loop_ _publ_author_name T.J.Boyle T.Q.Doan L.A.M.Steele C.Apblett S.M.Hoppe ; K.Hawthorne ; R.M.Kalinich W.M.Sigmund data_9ma052s _database_code_depnum_ccdc_archive 'CCDC 843197' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 N2 O2 Sn2' _chemical_formula_weight 539.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.984(3) _cell_length_b 7.4491(7) _cell_length_c 21.522(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.458(2) _cell_angle_gamma 90.00 _cell_volume 4148.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4646 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 25.24 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.128 _exptl_crystal_size_min 0.106 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 2.419 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_T_max 0.774 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14471 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.28 _reflns_number_total 3743 _reflns_number_gt 3353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3743 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.344734(11) 0.80277(4) 0.056814(14) 0.03169(10) Uani 1 1 d . . . Sn2 Sn 0.437568(11) 0.51921(4) 0.051290(14) 0.03083(10) Uani 1 1 d . . . N1 N 0.38540(13) 0.5718(5) 0.11416(16) 0.0318(8) Uani 1 1 d . . . N2 N 0.41988(13) 0.8072(4) 0.03104(15) 0.0289(8) Uani 1 1 d . . . O1 O 0.32243(11) 0.6075(4) -0.01419(13) 0.0361(7) Uani 1 1 d . . . O2 O 0.50225(10) 0.5869(4) 0.12497(14) 0.0388(7) Uani 1 1 d . . . C1 C 0.29008(14) 0.6218(5) -0.07489(19) 0.0280(9) Uani 1 1 d . . . C2 C 0.27643(17) 0.7859(5) -0.1051(2) 0.0375(10) Uani 1 1 d . . . H2 H 0.2893 0.8934 -0.0826 0.045 Uiso 1 1 calc R . . C3 C 0.24402(18) 0.7950(6) -0.1684(2) 0.0438(11) Uani 1 1 d . . . H3 H 0.2350 0.9080 -0.1889 0.053 Uiso 1 1 calc R . . C4 C 0.22523(17) 0.6386(7) -0.2009(2) 0.0437(11) Uani 1 1 d . . . H4 H 0.2034 0.6432 -0.2441 0.052 Uiso 1 1 calc R . . C5 C 0.23827(17) 0.4768(6) -0.1706(2) 0.0399(11) Uani 1 1 d . . . H5 H 0.2247 0.3702 -0.1934 0.048 Uiso 1 1 calc R . . C6 C 0.27060(15) 0.4627(5) -0.1079(2) 0.0294(9) Uani 1 1 d . . . C7 C 0.28498(18) 0.2851(5) -0.0751(2) 0.0401(11) Uani 1 1 d . . . H7A H 0.2670 0.2696 -0.0418 0.060 Uiso 1 1 calc R . . H7B H 0.3224 0.2810 -0.0548 0.060 Uiso 1 1 calc R . . H7C H 0.2750 0.1885 -0.1071 0.060 Uiso 1 1 calc R . . C8 C 0.53641(16) 0.4589(6) 0.1538(2) 0.0355(10) Uani 1 1 d . . . C9 C 0.52098(17) 0.2967(6) 0.1738(2) 0.0412(11) Uani 1 1 d . . . H9 H 0.4852 0.2741 0.1672 0.049 Uiso 1 1 calc R . . C10 C 0.5568(2) 0.1666(7) 0.2034(2) 0.0524(13) Uani 1 1 d . . . H10 H 0.5456 0.0560 0.2168 0.063 Uiso 1 1 calc R . . C11 C 0.6084(2) 0.1997(8) 0.2130(2) 0.0594(16) Uani 1 1 d . . . H11 H 0.6332 0.1104 0.2320 0.071 Uiso 1 1 calc R . . C12 C 0.62438(18) 0.3625(8) 0.1949(2) 0.0533(14) Uani 1 1 d . . . H12 H 0.6603 0.3852 0.2032 0.064 Uiso 1 1 calc R . . C13 C 0.58944(16) 0.4938(6) 0.1648(2) 0.0405(12) Uani 1 1 d . . . C14 C 0.60622(18) 0.6715(7) 0.1458(2) 0.0519(13) Uani 1 1 d . . . H14A H 0.6440 0.6783 0.1596 0.078 Uiso 1 1 calc R . . H14B H 0.5920 0.7677 0.1666 0.078 Uiso 1 1 calc R . . H14C H 0.5937 0.6850 0.0986 0.078 Uiso 1 1 calc R . . C15 C 0.41173(18) 0.6300(7) 0.1812(2) 0.0450(12) Uani 1 1 d . . . H15A H 0.3859 0.6677 0.2026 0.067 Uiso 1 1 calc R . . H15B H 0.4348 0.7309 0.1801 0.067 Uiso 1 1 calc R . . H15C H 0.4319 0.5300 0.2052 0.067 Uiso 1 1 calc R . . C16 C 0.35333(17) 0.4137(6) 0.1161(2) 0.0457(12) Uani 1 1 d . . . H16A H 0.3754 0.3146 0.1377 0.069 Uiso 1 1 calc R . . H16B H 0.3347 0.3780 0.0718 0.069 Uiso 1 1 calc R . . H16C H 0.3284 0.4429 0.1400 0.069 Uiso 1 1 calc R . . C17 C 0.41298(18) 0.8478(6) -0.0385(2) 0.0428(11) Uani 1 1 d . . . H17A H 0.3992 0.9695 -0.0482 0.064 Uiso 1 1 calc R . . H17B H 0.3888 0.7613 -0.0654 0.064 Uiso 1 1 calc R . . H17C H 0.4464 0.8393 -0.0479 0.064 Uiso 1 1 calc R . . C18 C 0.45636(19) 0.9364(6) 0.0705(2) 0.0459(12) Uani 1 1 d . . . H18A H 0.4905 0.9192 0.0638 0.069 Uiso 1 1 calc R . . H18B H 0.4587 0.9179 0.1164 0.069 Uiso 1 1 calc R . . H18C H 0.4443 1.0587 0.0578 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.03045(17) 0.03193(18) 0.03100(17) -0.00011(12) 0.00598(12) 0.00273(12) Sn2 0.02959(17) 0.03074(17) 0.02915(17) -0.00342(12) 0.00346(12) 0.00090(12) N1 0.0307(19) 0.034(2) 0.0288(19) 0.0055(15) 0.0056(15) -0.0026(15) N2 0.0324(18) 0.0290(19) 0.0232(18) -0.0015(14) 0.0043(15) -0.0079(14) O1 0.0387(17) 0.0266(15) 0.0345(17) 0.0033(13) -0.0033(13) -0.0004(13) O2 0.0271(15) 0.0424(18) 0.0421(18) -0.0056(14) 0.0020(13) 0.0027(13) C1 0.022(2) 0.028(2) 0.030(2) 0.0030(17) 0.0000(17) 0.0018(16) C2 0.038(2) 0.026(2) 0.042(3) -0.0053(19) 0.002(2) 0.0015(19) C3 0.041(3) 0.044(3) 0.043(3) 0.009(2) 0.005(2) 0.011(2) C4 0.035(2) 0.058(3) 0.030(2) -0.003(2) -0.0058(19) 0.002(2) C5 0.035(2) 0.040(3) 0.041(3) -0.011(2) 0.004(2) -0.007(2) C6 0.022(2) 0.031(2) 0.035(2) -0.0051(18) 0.0079(18) -0.0006(17) C7 0.045(3) 0.029(2) 0.046(3) -0.002(2) 0.013(2) -0.006(2) C8 0.030(2) 0.045(3) 0.028(2) -0.012(2) 0.0020(18) 0.005(2) C9 0.032(2) 0.052(3) 0.032(2) -0.009(2) -0.0021(19) 0.002(2) C10 0.058(3) 0.046(3) 0.039(3) -0.007(2) -0.008(2) 0.010(2) C11 0.049(3) 0.072(4) 0.042(3) -0.017(3) -0.012(2) 0.033(3) C12 0.026(2) 0.082(4) 0.044(3) -0.027(3) -0.003(2) 0.012(3) C13 0.029(2) 0.062(3) 0.028(2) -0.023(2) 0.0039(19) -0.001(2) C14 0.037(3) 0.074(4) 0.044(3) -0.020(3) 0.011(2) -0.016(2) C15 0.047(3) 0.062(3) 0.025(2) 0.004(2) 0.008(2) 0.003(2) C16 0.042(3) 0.049(3) 0.045(3) 0.017(2) 0.010(2) -0.005(2) C17 0.045(3) 0.046(3) 0.038(3) 0.005(2) 0.014(2) -0.004(2) C18 0.050(3) 0.040(3) 0.043(3) -0.005(2) 0.005(2) -0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.072(3) . ? Sn1 N1 2.218(3) . ? Sn1 N2 2.249(3) . ? Sn2 O2 2.061(3) . ? Sn2 N2 2.214(3) . ? Sn2 N1 2.246(3) . ? N1 C16 1.470(5) . ? N1 C15 1.481(5) . ? N2 C18 1.464(5) . ? N2 C17 1.486(5) . ? O1 C1 1.354(5) . ? O2 C8 1.349(5) . ? C1 C2 1.385(5) . ? C1 C6 1.405(5) . ? C2 C3 1.396(6) . ? C2 H2 0.9500 . ? C3 C4 1.379(6) . ? C3 H3 0.9500 . ? C4 C5 1.368(6) . ? C4 H4 0.9500 . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 C7 1.499(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.386(6) . ? C8 C13 1.407(6) . ? C9 C10 1.388(6) . ? C9 H9 0.9500 . ? C10 C11 1.373(7) . ? C10 H10 0.9500 . ? C11 C12 1.379(8) . ? C11 H11 0.9500 . ? C12 C13 1.385(7) . ? C12 H12 0.9500 . ? C13 C14 1.494(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 N1 81.98(12) . . ? O1 Sn1 N2 85.54(11) . . ? N1 Sn1 N2 79.06(12) . . ? O2 Sn2 N2 90.16(12) . . ? O2 Sn2 N1 91.86(12) . . ? N2 Sn2 N1 79.20(12) . . ? C16 N1 C15 109.3(3) . . ? C16 N1 Sn1 115.8(3) . . ? C15 N1 Sn1 109.9(3) . . ? C16 N1 Sn2 110.6(3) . . ? C15 N1 Sn2 115.4(3) . . ? Sn1 N1 Sn2 95.50(12) . . ? C18 N2 C17 108.8(3) . . ? C18 N2 Sn2 116.8(3) . . ? C17 N2 Sn2 110.7(3) . . ? C18 N2 Sn1 111.8(3) . . ? C17 N2 Sn1 112.8(3) . . ? Sn2 N2 Sn1 95.52(12) . . ? C1 O1 Sn1 129.0(2) . . ? C8 O2 Sn2 120.1(3) . . ? O1 C1 C2 122.4(4) . . ? O1 C1 C6 117.9(3) . . ? C2 C1 C6 119.7(4) . . ? C1 C2 C3 120.7(4) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 119.5(4) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 122.4(4) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 118.0(4) . . ? C5 C6 C7 122.2(4) . . ? C1 C6 C7 119.8(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C8 C9 122.2(4) . . ? O2 C8 C13 118.5(4) . . ? C9 C8 C13 119.3(4) . . ? C8 C9 C10 121.3(5) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C11 C10 C9 119.2(5) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 120.0(5) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 121.8(5) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C12 C13 C8 118.3(5) . . ? C12 C13 C14 122.3(4) . . ? C8 C13 C14 119.4(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.759 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.102 #===END data_9dc012s _database_code_depnum_ccdc_archive 'CCDC 843198' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 N2 O Sn' _chemical_formula_weight 377.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1411(12) _cell_length_b 9.4382(14) _cell_length_c 11.1451(17) _cell_angle_alpha 85.095(2) _cell_angle_beta 82.534(2) _cell_angle_gamma 88.505(2) _cell_volume 845.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5240 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.29 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 1.508 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 0.740 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6108 _diffrn_reflns_av_R_equivalents 0.0112 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.29 _reflns_number_total 3033 _reflns_number_gt 2973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.3952P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3033 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0201 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.292877(16) 0.456575(14) 1.012376(11) 0.02682(6) Uani 1 1 d . . . N1 N 0.4839(2) 0.62383(18) 0.91303(15) 0.0281(4) Uani 1 1 d . . . C16 C 0.0584(4) 0.2282(3) 0.2196(2) 0.0489(7) Uani 1 1 d . . . H16 H 0.0483 0.3197 0.2495 0.059 Uiso 1 1 calc R . . O1 O 0.35413(18) 0.33065(15) 0.86924(12) 0.0286(3) Uani 1 1 d . . . C1 C 0.2755(2) 0.3360(2) 0.76970(18) 0.0249(4) Uani 1 1 d . . . C2 C 0.3620(3) 0.2905(2) 0.66128(18) 0.0270(4) Uani 1 1 d . . . C3 C 0.2792(3) 0.2959(2) 0.5591(2) 0.0345(5) Uani 1 1 d . . . H3 H 0.3360 0.2656 0.4855 0.041 Uiso 1 1 calc R . . C4 C 0.1163(3) 0.3442(3) 0.5615(2) 0.0397(5) Uani 1 1 d . . . H4 H 0.0631 0.3477 0.4903 0.048 Uiso 1 1 calc R . . C5 C 0.0327(3) 0.3870(2) 0.6681(2) 0.0388(5) Uani 1 1 d . . . H5 H -0.0791 0.4194 0.6709 0.047 Uiso 1 1 calc R . . C6 C 0.1111(3) 0.3829(2) 0.7711(2) 0.0325(5) Uani 1 1 d . . . H6 H 0.0522 0.4125 0.8442 0.039 Uiso 1 1 calc R . . C7 C 0.5364(3) 0.2304(2) 0.66044(19) 0.0327(5) Uani 1 1 d . . . H7 H 0.5876 0.2758 0.7242 0.039 Uiso 1 1 calc R . . C8 C 0.5295(4) 0.0720(3) 0.6970(3) 0.0641(9) Uani 1 1 d . . . H8A H 0.4626 0.0553 0.7764 0.096 Uiso 1 1 calc . . . H8B H 0.6420 0.0344 0.7018 0.096 Uiso 1 1 calc . . . H8C H 0.4795 0.0240 0.6365 0.096 Uiso 1 1 calc . . . C9 C 0.6464(3) 0.2629(4) 0.5406(3) 0.0559(7) Uani 1 1 d . . . H9A H 0.6054 0.2128 0.4772 0.084 Uiso 1 1 calc . . . H9B H 0.7602 0.2313 0.5493 0.084 Uiso 1 1 calc . . . H9C H 0.6445 0.3656 0.5181 0.084 Uiso 1 1 calc . . . C10 C 0.5051(3) 0.6277(3) 0.7797(2) 0.0418(6) Uani 1 1 d . . . H10A H 0.3972 0.6436 0.7505 0.063 Uiso 1 1 calc . . . H10B H 0.5528 0.5370 0.7543 0.063 Uiso 1 1 calc . . . H10C H 0.5794 0.7051 0.7456 0.063 Uiso 1 1 calc . . . C11 C 0.4166(3) 0.7630(2) 0.9501(2) 0.0373(5) Uani 1 1 d . . . H11A H 0.4925 0.8384 0.9140 0.056 Uiso 1 1 calc . . . H11B H 0.4046 0.7621 1.0388 0.056 Uiso 1 1 calc . . . H11C H 0.3081 0.7804 0.9221 0.056 Uiso 1 1 calc . . . C12 C -0.0325(4) 0.1192(3) 0.2839(3) 0.0535(7) Uani 1 1 d . . . H12 H -0.1036 0.1358 0.3561 0.064 Uiso 1 1 calc R . . C13 C -0.0187(3) -0.0139(3) 0.2419(2) 0.0450(6) Uani 1 1 d . . . H13 H -0.0791 -0.0915 0.2845 0.054 Uiso 1 1 calc R . . C14 C 0.0852(3) -0.0314(3) 0.1365(2) 0.0453(6) Uani 1 1 d . . . H14 H 0.0975 -0.1219 0.1048 0.054 Uiso 1 1 calc R . . C15 C 0.1712(3) 0.0837(3) 0.0772(2) 0.0413(6) Uani 1 1 d . . . H15 H 0.2418 0.0703 0.0041 0.050 Uiso 1 1 calc R . . N2 N 0.1599(3) 0.2123(2) 0.11766(18) 0.0390(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.03068(10) 0.02614(9) 0.02257(9) -0.00510(6) 0.00238(6) 0.00082(6) N1 0.0384(10) 0.0258(9) 0.0199(8) -0.0005(6) -0.0038(7) -0.0013(7) C16 0.0624(17) 0.0318(13) 0.0481(15) -0.0093(11) 0.0149(13) -0.0056(12) O1 0.0322(8) 0.0317(8) 0.0228(7) -0.0077(6) -0.0045(6) 0.0051(6) C1 0.0295(10) 0.0193(9) 0.0257(10) -0.0008(7) -0.0033(8) -0.0023(8) C2 0.0318(11) 0.0243(10) 0.0244(10) -0.0009(8) -0.0026(8) -0.0031(8) C3 0.0426(13) 0.0374(12) 0.0236(11) -0.0013(9) -0.0042(9) -0.0041(10) C4 0.0473(14) 0.0397(13) 0.0347(12) 0.0014(10) -0.0180(11) -0.0005(10) C5 0.0353(12) 0.0335(12) 0.0500(15) -0.0045(10) -0.0144(11) 0.0057(10) C6 0.0324(11) 0.0278(11) 0.0376(12) -0.0072(9) -0.0036(9) 0.0027(9) C7 0.0300(11) 0.0422(13) 0.0265(11) -0.0097(9) -0.0015(9) 0.0002(9) C8 0.0467(16) 0.0504(17) 0.092(2) 0.0063(16) -0.0082(16) 0.0158(13) C9 0.0379(14) 0.087(2) 0.0409(15) -0.0144(14) 0.0076(11) -0.0040(14) C10 0.0572(15) 0.0462(14) 0.0217(11) 0.0053(10) -0.0061(10) -0.0149(12) C11 0.0433(13) 0.0264(11) 0.0434(13) -0.0011(10) -0.0125(10) 0.0041(10) C12 0.0595(17) 0.0447(15) 0.0493(16) -0.0075(12) 0.0227(13) -0.0072(13) C13 0.0438(14) 0.0356(13) 0.0524(15) 0.0012(11) 0.0040(12) -0.0093(11) C14 0.0456(14) 0.0350(13) 0.0556(16) -0.0142(11) -0.0003(12) -0.0053(11) C15 0.0389(13) 0.0442(14) 0.0400(13) -0.0127(11) 0.0048(10) -0.0066(11) N2 0.0433(11) 0.0349(11) 0.0368(11) -0.0066(8) 0.0066(9) -0.0075(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.0719(14) . ? Sn1 N1 2.1871(18) 2_667 ? Sn1 N1 2.3489(18) . ? N1 C10 1.470(3) . ? N1 C11 1.480(3) . ? N1 Sn1 2.1871(18) 2_667 ? C16 N2 1.332(3) . ? C16 C12 1.377(4) . ? C16 H16 0.9500 . ? O1 C1 1.347(2) . ? C1 C6 1.398(3) . ? C1 C2 1.411(3) . ? C2 C3 1.393(3) . ? C2 C7 1.514(3) . ? C3 C4 1.389(3) . ? C3 H3 0.9500 . ? C4 C5 1.377(4) . ? C4 H4 0.9500 . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.516(4) . ? C7 C9 1.521(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.375(4) . ? C12 H12 0.9500 . ? C13 C14 1.375(4) . ? C13 H13 0.9500 . ? C14 C15 1.380(4) . ? C14 H14 0.9500 . ? C15 N2 1.328(3) . ? C15 H15 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 N1 88.58(6) . 2_667 ? O1 Sn1 N1 88.34(6) . . ? N1 Sn1 N1 80.57(7) 2_667 . ? C10 N1 C11 108.91(18) . . ? C10 N1 Sn1 111.59(15) . 2_667 ? C11 N1 Sn1 117.01(13) . 2_667 ? C10 N1 Sn1 114.84(13) . . ? C11 N1 Sn1 104.79(13) . . ? Sn1 N1 Sn1 99.43(6) 2_667 . ? N2 C16 C12 123.6(2) . . ? N2 C16 H16 118.2 . . ? C12 C16 H16 118.2 . . ? C1 O1 Sn1 124.41(12) . . ? O1 C1 C6 122.14(19) . . ? O1 C1 C2 118.64(18) . . ? C6 C1 C2 119.21(19) . . ? C3 C2 C1 118.1(2) . . ? C3 C2 C7 121.98(19) . . ? C1 C2 C7 119.81(18) . . ? C4 C3 C2 122.0(2) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.1(2) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 121.2(2) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C2 C7 C8 109.49(19) . . ? C2 C7 C9 113.7(2) . . ? C8 C7 C9 111.6(2) . . ? C2 C7 H7 107.2 . . ? C8 C7 H7 107.2 . . ? C9 C7 H7 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C16 118.9(2) . . ? C13 C12 H12 120.6 . . ? C16 C12 H12 120.6 . . ? C12 C13 C14 118.0(2) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? C13 C14 C15 119.4(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? N2 C15 C14 123.0(2) . . ? N2 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C15 N2 C16 117.1(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.29 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.653 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.067 # start Validation Reply Form _vrf_PLAT780_9dc012s ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: py in lattice is not bound to the molecule. The remaining atoms form a connected set ; # end Validation Reply Form #===END data_9ag141s _database_code_depnum_ccdc_archive 'CCDC 843199' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H38 N2 O2 Sn2' _chemical_formula_weight 623.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2967(7) _cell_length_b 11.3895(9) _cell_length_c 21.6629(18) _cell_angle_alpha 89.6130(10) _cell_angle_beta 80.5720(10) _cell_angle_gamma 79.6220(10) _cell_volume 1985.8(3) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4363 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 24.77 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.224 _exptl_crystal_size_mid 0.198 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.907 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.659 _exptl_absorpt_correction_T_max 0.723 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14453 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7101 _reflns_number_gt 5975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.5726P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7101 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn -0.00957(4) 0.52989(3) 0.077822(14) 0.03450(9) Uani 1 1 d . . . Sn2 Sn 0.01255(3) 0.38394(2) 0.386066(13) 0.02472(8) Uani 1 1 d . . . Sn3 Sn 0.13438(3) 0.32085(2) 0.232945(13) 0.02569(8) Uani 1 1 d . . . N1 N 0.2387(4) 0.2926(3) 0.32180(15) 0.0258(8) Uani 1 1 d . . . N2 N -0.0334(4) 0.4655(3) 0.29231(16) 0.0280(8) Uani 1 1 d . . . N3 N -0.1335(4) 0.5994(3) -0.00255(17) 0.0371(9) Uani 1 1 d . . . O1 O 0.1262(3) 0.5265(2) 0.40328(12) 0.0266(6) Uani 1 1 d . . . O2 O -0.0271(3) 0.2075(2) 0.26656(12) 0.0292(6) Uani 1 1 d . . . O3 O 0.1569(4) 0.6442(3) 0.06058(13) 0.0366(7) Uani 1 1 d . . . C1 C 0.0418(5) 0.6263(3) 0.43616(17) 0.0244(9) Uani 1 1 d . . . C2 C -0.1267(5) 0.6363(4) 0.46158(18) 0.0288(9) Uani 1 1 d . . . H2 H -0.1804 0.5706 0.4570 0.035 Uiso 1 1 calc R . . C3 C -0.2184(5) 0.7387(4) 0.49326(19) 0.0328(10) Uani 1 1 d . . . H3 H -0.3321 0.7423 0.5106 0.039 Uiso 1 1 calc R . . C4 C -0.1423(5) 0.8345(4) 0.4992(2) 0.0327(10) Uani 1 1 d . . . H4 H -0.2042 0.9065 0.5191 0.039 Uiso 1 1 calc R . . C5 C 0.0262(5) 0.8255(3) 0.47575(18) 0.0286(9) Uani 1 1 d . . . H5 H 0.0779 0.8918 0.4812 0.034 Uiso 1 1 calc R . . C6 C 0.1222(5) 0.7232(3) 0.44467(17) 0.0232(9) Uani 1 1 d . . . C7 C 0.3103(5) 0.7160(3) 0.42318(18) 0.0251(9) Uani 1 1 d . . . C8 C 0.3560(5) 0.6992(4) 0.35160(19) 0.0325(10) Uani 1 1 d . . . H8A H 0.2960 0.7669 0.3314 0.049 Uiso 1 1 calc R . . H8B H 0.3251 0.6251 0.3388 0.049 Uiso 1 1 calc R . . H8C H 0.4759 0.6950 0.3390 0.049 Uiso 1 1 calc R . . C9 C 0.4057(5) 0.6108(4) 0.4546(2) 0.0348(10) Uani 1 1 d . . . H9A H 0.5250 0.6036 0.4393 0.052 Uiso 1 1 calc R . . H9B H 0.3694 0.5370 0.4445 0.052 Uiso 1 1 calc R . . H9C H 0.3837 0.6245 0.5000 0.052 Uiso 1 1 calc R . . C10 C 0.3692(5) 0.8291(4) 0.4405(2) 0.0348(10) Uani 1 1 d . . . H10A H 0.4898 0.8194 0.4275 0.052 Uiso 1 1 calc R . . H10B H 0.3417 0.8432 0.4859 0.052 Uiso 1 1 calc R . . H10C H 0.3140 0.8973 0.4193 0.052 Uiso 1 1 calc R . . C11 C -0.1434(5) 0.1792(3) 0.23451(18) 0.0267(9) Uani 1 1 d . . . C12 C -0.1903(5) 0.2498(4) 0.18511(19) 0.0332(10) Uani 1 1 d . . . H12 H -0.1396 0.3172 0.1745 0.040 Uiso 1 1 calc R . . C13 C -0.3079(6) 0.2249(4) 0.1512(2) 0.0408(11) Uani 1 1 d . . . H13 H -0.3371 0.2740 0.1176 0.049 Uiso 1 1 calc R . . C14 C -0.3814(6) 0.1278(4) 0.1669(2) 0.0423(12) Uani 1 1 d . . . H14 H -0.4630 0.1092 0.1444 0.051 Uiso 1 1 calc R . . C15 C -0.3367(5) 0.0568(4) 0.2158(2) 0.0370(11) Uani 1 1 d . . . H15 H -0.3888 -0.0103 0.2256 0.044 Uiso 1 1 calc R . . C16 C -0.2193(5) 0.0790(3) 0.25106(19) 0.0277(9) Uani 1 1 d . . . C17 C -0.1766(5) 0.0008(4) 0.3060(2) 0.0339(10) Uani 1 1 d . . . C18 C 0.0073(5) -0.0592(4) 0.2940(2) 0.0416(12) Uani 1 1 d . . . H18A H 0.0276 -0.1153 0.2582 0.062 Uiso 1 1 calc R . . H18B H 0.0349 -0.1025 0.3312 0.062 Uiso 1 1 calc R . . H18C H 0.0769 0.0018 0.2848 0.062 Uiso 1 1 calc R . . C19 C -0.2790(6) -0.1004(4) 0.3157(2) 0.0521(14) Uani 1 1 d . . . H19A H -0.3972 -0.0658 0.3267 0.078 Uiso 1 1 calc R . . H19B H -0.2439 -0.1512 0.3495 0.078 Uiso 1 1 calc R . . H19C H -0.2607 -0.1483 0.2769 0.078 Uiso 1 1 calc R . . C20 C -0.2162(6) 0.0769(4) 0.3668(2) 0.0424(12) Uani 1 1 d . . . H20A H -0.1493 0.1400 0.3629 0.064 Uiso 1 1 calc R . . H20B H -0.1901 0.0261 0.4019 0.064 Uiso 1 1 calc R . . H20C H -0.3344 0.1129 0.3745 0.064 Uiso 1 1 calc R . . C21 C 0.3908(5) 0.3456(4) 0.3168(2) 0.0340(10) Uani 1 1 d . . . H21A H 0.4312 0.3393 0.3570 0.051 Uiso 1 1 calc R . . H21B H 0.3651 0.4298 0.3060 0.051 Uiso 1 1 calc R . . H21C H 0.4766 0.3027 0.2842 0.051 Uiso 1 1 calc R . . C22 C 0.2810(5) 0.1645(4) 0.3364(2) 0.0350(10) Uani 1 1 d . . . H22A H 0.3535 0.1213 0.3003 0.053 Uiso 1 1 calc R . . H22B H 0.1789 0.1312 0.3459 0.053 Uiso 1 1 calc R . . H22C H 0.3385 0.1562 0.3727 0.053 Uiso 1 1 calc R . . C23 C 0.0161(6) 0.5821(4) 0.2783(2) 0.0396(11) Uani 1 1 d . . . H23A H -0.0131 0.6090 0.2378 0.059 Uiso 1 1 calc R . . H23B H 0.1364 0.5743 0.2766 0.059 Uiso 1 1 calc R . . H23C H -0.0419 0.6407 0.3111 0.059 Uiso 1 1 calc R . . C24 C -0.2139(5) 0.4779(4) 0.2908(2) 0.0435(12) Uani 1 1 d . . . H24A H -0.2759 0.5393 0.3215 0.065 Uiso 1 1 calc R . . H24B H -0.2494 0.4015 0.3009 0.065 Uiso 1 1 calc R . . H24C H -0.2357 0.5012 0.2489 0.065 Uiso 1 1 calc R . . C25 C 0.2615(5) 0.6562(4) 0.10183(19) 0.0305(10) Uani 1 1 d . . . C26 C 0.3409(6) 0.5554(4) 0.1290(2) 0.0405(11) Uani 1 1 d . . . H26 H 0.3192 0.4792 0.1192 0.049 Uiso 1 1 calc R . . C27 C 0.4510(6) 0.5636(5) 0.1699(2) 0.0472(13) Uani 1 1 d . . . H27 H 0.5043 0.4938 0.1877 0.057 Uiso 1 1 calc R . . C28 C 0.4819(6) 0.6731(5) 0.1844(2) 0.0481(13) Uani 1 1 d . . . H28 H 0.5564 0.6802 0.2125 0.058 Uiso 1 1 calc R . . C29 C 0.4036(6) 0.7731(4) 0.1577(2) 0.0445(12) Uani 1 1 d . . . H29 H 0.4267 0.8486 0.1681 0.053 Uiso 1 1 calc R . . C30 C 0.2927(5) 0.7694(4) 0.1163(2) 0.0339(10) Uani 1 1 d . . . C31 C 0.2117(7) 0.8831(4) 0.0867(2) 0.0540(15) Uani 1 1 d . . . C32 C 0.2657(8) 0.8726(5) 0.0154(3) 0.0663(17) Uani 1 1 d . . . H32A H 0.3864 0.8672 0.0053 0.099 Uiso 1 1 calc R . . H32B H 0.2103 0.9432 -0.0040 0.099 Uiso 1 1 calc R . . H32C H 0.2349 0.8008 -0.0004 0.099 Uiso 1 1 calc R . . C33 C 0.0218(7) 0.9000(5) 0.1037(3) 0.076(2) Uani 1 1 d . . . H33A H -0.0165 0.8311 0.0881 0.114 Uiso 1 1 calc R . . H33B H -0.0288 0.9728 0.0847 0.114 Uiso 1 1 calc R . . H33C H -0.0106 0.9070 0.1493 0.114 Uiso 1 1 calc R . . C34 C 0.2653(10) 0.9940(5) 0.1097(3) 0.107(3) Uani 1 1 d . . . H34A H 0.2392 0.9997 0.1554 0.160 Uiso 1 1 calc R . . H34B H 0.2061 1.0651 0.0919 0.160 Uiso 1 1 calc R . . H34C H 0.3853 0.9884 0.0964 0.160 Uiso 1 1 calc R . . C35 C -0.1180(8) 0.7215(4) -0.0218(3) 0.0652(17) Uani 1 1 d . . . H35A H -0.1677 0.7397 -0.0596 0.098 Uiso 1 1 calc R . . H35B H -0.0002 0.7279 -0.0306 0.098 Uiso 1 1 calc R . . H35C H -0.1756 0.7783 0.0119 0.098 Uiso 1 1 calc R . . C36 C -0.3129(6) 0.5922(6) 0.0150(3) 0.0676(18) Uani 1 1 d . . . H36A H -0.3609 0.6418 0.0526 0.101 Uiso 1 1 calc R . . H36B H -0.3241 0.5091 0.0233 0.101 Uiso 1 1 calc R . . H36C H -0.3716 0.6209 -0.0195 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.03206(18) 0.03882(19) 0.03212(18) 0.00401(14) -0.00041(13) -0.00964(14) Sn2 0.02141(15) 0.02552(16) 0.02707(16) -0.00394(12) -0.00231(11) -0.00515(11) Sn3 0.02685(16) 0.02590(16) 0.02437(16) -0.00115(11) -0.00239(12) -0.00649(12) N1 0.0220(18) 0.0246(18) 0.0296(19) -0.0044(15) -0.0039(15) -0.0010(14) N2 0.0270(19) 0.0255(18) 0.034(2) -0.0026(15) -0.0113(15) -0.0042(15) N3 0.033(2) 0.039(2) 0.039(2) -0.0014(17) -0.0073(17) -0.0043(17) O1 0.0224(15) 0.0261(15) 0.0315(16) -0.0076(12) -0.0029(12) -0.0061(12) O2 0.0332(16) 0.0299(16) 0.0296(16) 0.0040(12) -0.0106(13) -0.0141(13) O3 0.0427(19) 0.0347(17) 0.0379(18) 0.0047(14) -0.0131(15) -0.0160(14) C1 0.028(2) 0.028(2) 0.016(2) -0.0015(16) -0.0051(17) -0.0022(18) C2 0.025(2) 0.038(2) 0.027(2) -0.0073(19) -0.0045(18) -0.0133(19) C3 0.024(2) 0.041(3) 0.031(2) -0.002(2) -0.0043(19) 0.000(2) C4 0.032(3) 0.027(2) 0.034(2) -0.0051(19) -0.0002(19) 0.0051(19) C5 0.033(2) 0.023(2) 0.028(2) 0.0007(17) -0.0020(19) -0.0039(18) C6 0.024(2) 0.029(2) 0.017(2) 0.0006(16) -0.0034(16) -0.0032(17) C7 0.024(2) 0.025(2) 0.026(2) 0.0014(17) -0.0017(17) -0.0052(17) C8 0.025(2) 0.035(2) 0.036(3) -0.0009(19) 0.0007(19) -0.0044(19) C9 0.026(2) 0.036(3) 0.045(3) 0.005(2) -0.010(2) -0.0093(19) C10 0.035(3) 0.038(3) 0.033(2) -0.004(2) -0.001(2) -0.013(2) C11 0.027(2) 0.027(2) 0.026(2) -0.0038(17) -0.0026(18) -0.0038(18) C12 0.041(3) 0.035(2) 0.028(2) 0.0055(19) -0.007(2) -0.015(2) C13 0.045(3) 0.047(3) 0.031(3) -0.001(2) -0.014(2) -0.003(2) C14 0.036(3) 0.049(3) 0.047(3) -0.011(2) -0.019(2) -0.009(2) C15 0.033(3) 0.035(3) 0.043(3) -0.008(2) -0.003(2) -0.010(2) C16 0.023(2) 0.026(2) 0.032(2) -0.0048(18) -0.0022(18) -0.0027(17) C17 0.034(3) 0.028(2) 0.041(3) 0.0053(19) -0.003(2) -0.0095(19) C18 0.041(3) 0.033(3) 0.051(3) 0.006(2) -0.009(2) -0.003(2) C19 0.049(3) 0.036(3) 0.069(4) 0.013(3) 0.001(3) -0.013(2) C20 0.047(3) 0.043(3) 0.034(3) 0.011(2) -0.003(2) -0.003(2) C21 0.022(2) 0.039(3) 0.042(3) -0.007(2) -0.0052(19) -0.0079(19) C22 0.035(3) 0.032(2) 0.034(3) -0.004(2) -0.004(2) 0.003(2) C23 0.055(3) 0.026(2) 0.038(3) -0.001(2) -0.015(2) -0.001(2) C24 0.031(3) 0.049(3) 0.048(3) -0.013(2) -0.014(2) 0.008(2) C25 0.027(2) 0.040(3) 0.024(2) 0.0019(19) -0.0001(18) -0.0085(19) C26 0.045(3) 0.032(3) 0.046(3) 0.008(2) -0.008(2) -0.011(2) C27 0.046(3) 0.056(3) 0.038(3) 0.011(2) -0.011(2) -0.002(3) C28 0.044(3) 0.068(4) 0.034(3) 0.000(3) -0.017(2) -0.003(3) C29 0.053(3) 0.045(3) 0.039(3) -0.007(2) -0.018(2) -0.007(2) C30 0.038(3) 0.034(2) 0.029(2) -0.0041(19) -0.005(2) -0.003(2) C31 0.082(4) 0.028(3) 0.058(4) -0.003(2) -0.040(3) -0.002(3) C32 0.093(5) 0.052(3) 0.067(4) 0.025(3) -0.038(4) -0.026(3) C33 0.087(5) 0.071(4) 0.061(4) -0.027(3) -0.037(3) 0.035(3) C34 0.189(8) 0.029(3) 0.129(6) 0.001(4) -0.103(6) -0.020(4) C35 0.104(5) 0.033(3) 0.067(4) 0.004(3) -0.050(4) -0.001(3) C36 0.029(3) 0.108(5) 0.061(4) -0.036(3) -0.004(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O3 2.053(3) . ? Sn1 N3 2.234(4) . ? Sn1 N3 2.237(4) 2_565 ? Sn2 O1 2.083(2) . ? Sn2 N1 2.237(3) . ? Sn2 N2 2.288(3) . ? Sn3 O2 2.069(3) . ? Sn3 N2 2.219(3) . ? Sn3 N1 2.235(3) . ? N1 C21 1.483(5) . ? N1 C22 1.483(5) . ? N2 C23 1.475(5) . ? N2 C24 1.484(5) . ? N3 C35 1.471(6) . ? N3 C36 1.492(6) . ? N3 Sn1 2.237(4) 2_565 ? O1 C1 1.360(4) . ? O2 C11 1.361(5) . ? O3 C25 1.367(5) . ? C1 C2 1.401(5) . ? C1 C6 1.416(5) . ? C2 C3 1.389(5) . ? C2 H2 0.9500 . ? C3 C4 1.371(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 H4 0.9500 . ? C5 C6 1.395(5) . ? C5 H5 0.9500 . ? C6 C7 1.541(5) . ? C7 C10 1.528(5) . ? C7 C9 1.533(5) . ? C7 C8 1.539(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.398(6) . ? C11 C16 1.417(5) . ? C12 C13 1.382(6) . ? C12 H12 0.9500 . ? C13 C14 1.372(6) . ? C13 H13 0.9500 . ? C14 C15 1.386(6) . ? C14 H14 0.9500 . ? C15 C16 1.390(6) . ? C15 H15 0.9500 . ? C16 C17 1.530(6) . ? C17 C18 1.537(6) . ? C17 C20 1.539(6) . ? C17 C19 1.544(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.394(6) . ? C25 C30 1.407(6) . ? C26 C27 1.389(6) . ? C26 H26 0.9500 . ? C27 C28 1.365(7) . ? C27 H27 0.9500 . ? C28 C29 1.379(6) . ? C28 H28 0.9500 . ? C29 C30 1.392(6) . ? C29 H29 0.9500 . ? C30 C31 1.535(6) . ? C31 C34 1.524(7) . ? C31 C32 1.534(7) . ? C31 C33 1.535(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sn1 N3 91.64(12) . . ? O3 Sn1 N3 92.61(12) . 2_565 ? N3 Sn1 N3 80.33(14) . 2_565 ? O1 Sn2 N1 92.29(11) . . ? O1 Sn2 N2 89.03(11) . . ? N1 Sn2 N2 78.74(12) . . ? O2 Sn3 N2 88.14(11) . . ? O2 Sn3 N1 87.55(11) . . ? N2 Sn3 N1 80.26(12) . . ? C21 N1 C22 108.7(3) . . ? C21 N1 Sn3 109.4(2) . . ? C22 N1 Sn3 112.6(2) . . ? C21 N1 Sn2 117.5(2) . . ? C22 N1 Sn2 111.3(2) . . ? Sn3 N1 Sn2 96.99(12) . . ? C23 N2 C24 108.5(3) . . ? C23 N2 Sn3 111.1(3) . . ? C24 N2 Sn3 116.9(2) . . ? C23 N2 Sn2 117.0(2) . . ? C24 N2 Sn2 107.3(3) . . ? Sn3 N2 Sn2 95.97(12) . . ? C35 N3 C36 109.3(4) . . ? C35 N3 Sn1 116.6(3) . . ? C36 N3 Sn1 106.9(3) . . ? C35 N3 Sn1 109.1(3) . 2_565 ? C36 N3 Sn1 115.2(3) . 2_565 ? Sn1 N3 Sn1 99.67(14) . 2_565 ? C1 O1 Sn2 122.4(2) . . ? C11 O2 Sn3 123.3(2) . . ? C25 O3 Sn1 120.8(2) . . ? O1 C1 C2 120.9(3) . . ? O1 C1 C6 120.6(3) . . ? C2 C1 C6 118.5(4) . . ? C3 C2 C1 122.4(4) . . ? C3 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? C4 C3 C2 119.0(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 122.7(4) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C1 117.7(4) . . ? C5 C6 C7 120.3(3) . . ? C1 C6 C7 122.0(3) . . ? C10 C7 C9 107.8(3) . . ? C10 C7 C8 107.0(3) . . ? C9 C7 C8 109.4(3) . . ? C10 C7 C6 112.2(3) . . ? C9 C7 C6 109.4(3) . . ? C8 C7 C6 110.9(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 C12 120.1(4) . . ? O2 C11 C16 120.6(4) . . ? C12 C11 C16 119.3(4) . . ? C13 C12 C11 122.3(4) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C14 C13 C12 118.6(4) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 123.2(4) . . ? C14 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C15 C16 C11 116.6(4) . . ? C15 C16 C17 121.8(4) . . ? C11 C16 C17 121.6(4) . . ? C16 C17 C18 110.7(3) . . ? C16 C17 C20 109.9(3) . . ? C18 C17 C20 110.3(4) . . ? C16 C17 C19 111.7(4) . . ? C18 C17 C19 106.8(4) . . ? C20 C17 C19 107.4(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 H23A 109.5 . . ? N2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 H24A 109.5 . . ? N2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 C26 120.0(4) . . ? O3 C25 C30 120.6(4) . . ? C26 C25 C30 119.4(4) . . ? C27 C26 C25 121.7(4) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C28 C27 C26 119.4(4) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 119.2(5) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C30 123.5(5) . . ? C28 C29 H29 118.2 . . ? C30 C29 H29 118.2 . . ? C29 C30 C25 116.8(4) . . ? C29 C30 C31 121.6(4) . . ? C25 C30 C31 121.7(4) . . ? C34 C31 C32 107.8(5) . . ? C34 C31 C30 111.7(4) . . ? C32 C31 C30 108.9(4) . . ? C34 C31 C33 107.8(5) . . ? C32 C31 C33 110.5(4) . . ? C30 C31 C33 110.1(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.756 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.097 #===END data_10oc131s _database_code_depnum_ccdc_archive 'CCDC 843200' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 N2 O2 Sn2' _chemical_formula_weight 567.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3543(19) _cell_length_b 14.471(2) _cell_length_c 13.135(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.226(3) _cell_angle_gamma 90.00 _cell_volume 2276.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3866 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 22.21 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 2.210 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.456 _exptl_absorpt_correction_T_max 0.643 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16132 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.28 _reflns_number_total 4132 _reflns_number_gt 3368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+1.0236P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4132 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.12479(3) 0.04870(2) 0.88060(3) 0.03767(12) Uani 1 1 d . . . Sn2 Sn 0.35900(3) 0.16997(3) 0.96472(3) 0.05507(15) Uani 1 1 d . . . N1 N 0.2669(4) 0.0564(3) 1.0231(3) 0.0475(11) Uani 1 1 d . . . N2 N 0.2573(4) 0.1115(3) 0.8149(3) 0.0522(11) Uani 1 1 d . . . O1 O 0.1640(3) -0.0829(2) 0.8430(3) 0.0483(9) Uani 1 1 d . . . O2 O 0.2246(3) 0.2525(2) 0.9679(3) 0.0524(9) Uani 1 1 d . . . C1 C 0.0779(4) -0.1441(3) 0.8068(4) 0.0449(13) Uani 1 1 d . . . C2 C 0.0528(5) -0.2090(4) 0.8764(4) 0.0502(14) Uani 1 1 d . . . C3 C -0.0328(5) -0.2721(4) 0.8392(6) 0.0635(17) Uani 1 1 d . . . H3 H -0.0496 -0.3175 0.8853 0.076 Uiso 1 1 calc R . . C4 C -0.0940(6) -0.2693(4) 0.7355(6) 0.0730(19) Uani 1 1 d . . . H4 H -0.1545 -0.3107 0.7111 0.088 Uiso 1 1 calc R . . C5 C -0.0661(5) -0.2064(5) 0.6686(5) 0.0662(17) Uani 1 1 d . . . H5 H -0.1067 -0.2059 0.5971 0.079 Uiso 1 1 calc R . . C6 C 0.0197(5) -0.1433(4) 0.7022(4) 0.0498(13) Uani 1 1 d . . . C7 C 0.0488(6) -0.0745(5) 0.6258(5) 0.0694(18) Uani 1 1 d . . . H7A H 0.0400 -0.0115 0.6499 0.104 Uiso 1 1 calc . . . H7B H -0.0011 -0.0836 0.5560 0.104 Uiso 1 1 calc . . . H7C H 0.1264 -0.0839 0.6222 0.104 Uiso 1 1 calc . . . C8 C 0.1181(6) -0.2099(5) 0.9889(5) 0.0713(18) Uani 1 1 d . . . H8A H 0.1979 -0.2152 0.9920 0.107 Uiso 1 1 calc . . . H8B H 0.0946 -0.2626 1.0251 0.107 Uiso 1 1 calc . . . H8C H 0.1044 -0.1524 1.0231 0.107 Uiso 1 1 calc . . . C9 C 0.2206(4) 0.3407(4) 1.0026(4) 0.0456(13) Uani 1 1 d . . . C10 C 0.1380(5) 0.3988(4) 0.9431(4) 0.0503(14) Uani 1 1 d . . . C11 C 0.1332(6) 0.4899(5) 0.9789(6) 0.073(2) Uani 1 1 d . . . H11 H 0.0789 0.5311 0.9395 0.088 Uiso 1 1 calc R . . C12 C 0.2058(8) 0.5208(5) 1.0702(6) 0.081(2) Uani 1 1 d . . . H12 H 0.2023 0.5829 1.0927 0.097 Uiso 1 1 calc R . . C13 C 0.2815(6) 0.4619(5) 1.1268(6) 0.0695(18) Uani 1 1 d . . . H13 H 0.3302 0.4836 1.1899 0.083 Uiso 1 1 calc R . . C14 C 0.2915(5) 0.3715(4) 1.0974(5) 0.0546(14) Uani 1 1 d . . . C15 C 0.3731(6) 0.3080(5) 1.1680(5) 0.087(2) Uani 1 1 d . . . H15A H 0.4387 0.2996 1.1396 0.130 Uiso 1 1 calc . . . H15B H 0.3376 0.2480 1.1721 0.130 Uiso 1 1 calc . . . H15C H 0.3962 0.3351 1.2384 0.130 Uiso 1 1 calc . . . C16 C 0.0587(5) 0.3651(5) 0.8453(5) 0.0706(18) Uani 1 1 d . . . H16A H 0.0962 0.3643 0.7877 0.106 Uiso 1 1 calc . . . H16B H -0.0061 0.4063 0.8273 0.106 Uiso 1 1 calc . . . H16C H 0.0339 0.3024 0.8568 0.106 Uiso 1 1 calc . . . C17 C 0.2113(7) 0.1810(5) 0.7327(5) 0.078(2) Uani 1 1 d . . . H17A H 0.2728 0.2131 0.7126 0.117 Uiso 1 1 calc . . . H17B H 0.1661 0.2259 0.7601 0.117 Uiso 1 1 calc . . . H17C H 0.1645 0.1500 0.6711 0.117 Uiso 1 1 calc . . . C18 C 0.3274(6) 0.0451(5) 0.7745(6) 0.079(2) Uani 1 1 d . . . H18A H 0.2862 0.0223 0.7055 0.118 Uiso 1 1 calc . . . H18B H 0.3465 -0.0070 0.8233 0.118 Uiso 1 1 calc . . . H18C H 0.3959 0.0758 0.7677 0.118 Uiso 1 1 calc . . . C19 C 0.3398(6) -0.0265(4) 1.0483(6) 0.080(2) Uani 1 1 d . . . H19A H 0.4029 -0.0128 1.1079 0.119 Uiso 1 1 calc . . . H19B H 0.3678 -0.0433 0.9871 0.119 Uiso 1 1 calc . . . H19C H 0.2966 -0.0781 1.0664 0.119 Uiso 1 1 calc . . . C20 C 0.2236(6) 0.0797(5) 1.1155(5) 0.0722(19) Uani 1 1 d . . . H20A H 0.1686 0.0332 1.1235 0.108 Uiso 1 1 calc . . . H20B H 0.1881 0.1407 1.1054 0.108 Uiso 1 1 calc . . . H20C H 0.2854 0.0804 1.1787 0.108 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0368(2) 0.0387(2) 0.0371(2) 0.00428(14) 0.00820(15) 0.00445(15) Sn2 0.0444(2) 0.0588(3) 0.0610(3) -0.00874(19) 0.01112(19) -0.00999(18) N1 0.044(3) 0.045(3) 0.048(3) 0.006(2) 0.001(2) 0.004(2) N2 0.059(3) 0.055(3) 0.048(3) -0.009(2) 0.023(2) -0.012(2) O1 0.047(2) 0.0368(19) 0.060(2) -0.0026(17) 0.0114(18) 0.0027(17) O2 0.050(2) 0.043(2) 0.053(2) -0.0031(17) -0.0080(17) -0.0028(17) C1 0.045(3) 0.032(3) 0.062(4) -0.001(2) 0.021(3) 0.007(2) C2 0.051(3) 0.044(3) 0.062(4) 0.001(3) 0.025(3) 0.009(3) C3 0.068(4) 0.038(3) 0.099(5) 0.001(3) 0.049(4) -0.001(3) C4 0.065(4) 0.057(4) 0.103(6) -0.027(4) 0.033(4) -0.021(3) C5 0.057(4) 0.077(5) 0.064(4) -0.019(3) 0.014(3) -0.007(3) C6 0.051(3) 0.049(3) 0.049(3) -0.007(3) 0.013(3) 0.003(3) C7 0.080(5) 0.076(4) 0.051(4) 0.009(3) 0.014(3) -0.001(4) C8 0.076(5) 0.077(4) 0.062(4) 0.025(3) 0.018(3) 0.011(4) C9 0.048(3) 0.042(3) 0.049(3) 0.001(2) 0.014(3) -0.007(2) C10 0.056(3) 0.051(3) 0.049(3) 0.016(3) 0.021(3) 0.001(3) C11 0.099(5) 0.063(4) 0.072(5) 0.025(4) 0.048(4) 0.032(4) C12 0.114(6) 0.056(4) 0.087(5) -0.015(4) 0.050(5) -0.003(4) C13 0.077(5) 0.063(4) 0.073(4) -0.022(4) 0.029(4) -0.012(4) C14 0.050(3) 0.057(4) 0.059(4) -0.016(3) 0.017(3) -0.013(3) C15 0.078(5) 0.089(5) 0.068(4) -0.022(4) -0.031(4) 0.007(4) C16 0.064(4) 0.079(5) 0.064(4) 0.020(3) 0.008(3) 0.009(4) C17 0.114(6) 0.072(4) 0.048(4) 0.007(3) 0.020(4) -0.036(4) C18 0.063(4) 0.100(6) 0.088(5) -0.034(4) 0.045(4) -0.026(4) C19 0.064(4) 0.055(4) 0.096(5) 0.004(4) -0.027(4) 0.013(3) C20 0.087(5) 0.086(5) 0.042(3) 0.003(3) 0.013(3) -0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.055(3) . ? Sn1 N2 2.224(4) . ? Sn1 N1 2.233(4) . ? Sn2 O2 2.054(4) . ? Sn2 N2 2.226(4) . ? Sn2 N1 2.238(4) . ? N1 C20 1.480(8) . ? N1 C19 1.488(7) . ? N2 C18 1.477(8) . ? N2 C17 1.482(8) . ? O1 C1 1.376(6) . ? O2 C9 1.361(6) . ? C1 C6 1.385(8) . ? C1 C2 1.397(7) . ? C2 C3 1.393(8) . ? C2 C8 1.499(8) . ? C3 C4 1.387(9) . ? C3 H3 0.9500 . ? C4 C5 1.366(9) . ? C4 H4 0.9500 . ? C5 C6 1.387(8) . ? C5 H5 0.9500 . ? C6 C7 1.519(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.401(7) . ? C9 C14 1.407(7) . ? C10 C11 1.406(9) . ? C10 C16 1.494(8) . ? C11 C12 1.384(10) . ? C11 H11 0.9500 . ? C12 C13 1.346(10) . ? C12 H12 0.9500 . ? C13 C14 1.378(8) . ? C13 H13 0.9500 . ? C14 C15 1.503(9) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 N2 92.64(16) . . ? O1 Sn1 N1 93.69(15) . . ? N2 Sn1 N1 78.62(17) . . ? O2 Sn2 N2 87.43(15) . . ? O2 Sn2 N1 86.46(15) . . ? N2 Sn2 N1 78.46(16) . . ? C20 N1 C19 108.8(5) . . ? C20 N1 Sn1 109.3(4) . . ? C19 N1 Sn1 117.0(4) . . ? C20 N1 Sn2 115.5(4) . . ? C19 N1 Sn2 109.8(4) . . ? Sn1 N1 Sn2 96.36(16) . . ? C18 N2 C17 109.5(5) . . ? C18 N2 Sn1 115.2(4) . . ? C17 N2 Sn1 111.9(4) . . ? C18 N2 Sn2 108.2(4) . . ? C17 N2 Sn2 114.7(4) . . ? Sn1 N2 Sn2 96.98(16) . . ? C1 O1 Sn1 118.1(3) . . ? C9 O2 Sn2 130.4(3) . . ? O1 C1 C6 120.4(5) . . ? O1 C1 C2 118.9(5) . . ? C6 C1 C2 120.6(5) . . ? C3 C2 C1 118.9(6) . . ? C3 C2 C8 121.2(5) . . ? C1 C2 C8 119.9(5) . . ? C4 C3 C2 120.6(6) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 119.3(6) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.8(6) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C1 C6 C5 118.7(6) . . ? C1 C6 C7 120.8(5) . . ? C5 C6 C7 120.5(6) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C10 117.2(5) . . ? O2 C9 C14 121.8(5) . . ? C10 C9 C14 120.9(5) . . ? C9 C10 C11 117.5(6) . . ? C9 C10 C16 121.2(5) . . ? C11 C10 C16 121.4(6) . . ? C12 C11 C10 121.4(6) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C13 C12 C11 119.2(6) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 123.0(7) . . ? C12 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C13 C14 C9 118.0(6) . . ? C13 C14 C15 120.0(6) . . ? C9 C14 C15 122.0(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 H20A 109.5 . . ? N1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.178 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.106 #===END data_9oc093s _database_code_depnum_ccdc_archive 'CCDC 843201' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H46 N2 O2 Sn2' _chemical_formula_weight 680.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9563(8) _cell_length_b 20.5582(17) _cell_length_c 15.2269(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.5180(10) _cell_angle_gamma 90.00 _cell_volume 3053.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5789 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.23 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.660 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.847 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21691 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.26 _reflns_number_total 5526 _reflns_number_gt 4934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+1.6841P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5526 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.103696(15) 0.479153(7) 0.779453(10) 0.02364(5) Uani 1 1 d . . . Sn2 Sn 0.428196(16) 0.439742(8) 0.785968(11) 0.02850(6) Uani 1 1 d . . . N1 N 0.3078(2) 0.52855(9) 0.80292(13) 0.0273(4) Uani 1 1 d . . . N2 N 0.22254(19) 0.40985(9) 0.71025(12) 0.0266(4) Uani 1 1 d . . . O1 O 0.36414(17) 0.40400(8) 0.89708(11) 0.0321(4) Uani 1 1 d . . . O2 O 0.03399(16) 0.52835(8) 0.66136(11) 0.0289(4) Uani 1 1 d . . . C1 C 0.3883(2) 0.35596(11) 0.95866(15) 0.0252(5) Uani 1 1 d . . . C2 C 0.3155(2) 0.35838(12) 1.02957(16) 0.0292(5) Uani 1 1 d . . . C3 C 0.3405(3) 0.31081(13) 1.09567(17) 0.0397(6) Uani 1 1 d . . . H3 H 0.2922 0.3122 1.1435 0.048 Uiso 1 1 calc R . . C4 C 0.4342(3) 0.26139(14) 1.09343(18) 0.0442(7) Uani 1 1 d . . . H4 H 0.4508 0.2296 1.1396 0.053 Uiso 1 1 calc R . . C5 C 0.5032(3) 0.25885(12) 1.02367(17) 0.0356(6) Uani 1 1 d . . . H5 H 0.5669 0.2247 1.0222 0.043 Uiso 1 1 calc R . . C6 C 0.4825(2) 0.30481(11) 0.95519(15) 0.0274(5) Uani 1 1 d . . . C7 C 0.5667(2) 0.30149(12) 0.88270(16) 0.0303(5) Uani 1 1 d . . . H7 H 0.5126 0.3236 0.8286 0.036 Uiso 1 1 calc R . . C8 C 0.6999(3) 0.33978(15) 0.91115(18) 0.0428(7) Uani 1 1 d . . . H8A H 0.6785 0.3852 0.9224 0.064 Uiso 1 1 calc . . . H8B H 0.7527 0.3380 0.8633 0.064 Uiso 1 1 calc . . . H8C H 0.7540 0.3207 0.9660 0.064 Uiso 1 1 calc . . . C9 C 0.5974(3) 0.23270(14) 0.8544(2) 0.0494(7) Uani 1 1 d . . . H9A H 0.6569 0.2106 0.9046 0.074 Uiso 1 1 calc . . . H9B H 0.6435 0.2349 0.8033 0.074 Uiso 1 1 calc . . . H9C H 0.5114 0.2085 0.8372 0.074 Uiso 1 1 calc . . . C10 C 0.2120(2) 0.41197(12) 1.03453(17) 0.0335(6) Uani 1 1 d . . . H10 H 0.2204 0.4446 0.9872 0.040 Uiso 1 1 calc R . . C11 C 0.0655(3) 0.38660(15) 1.0138(2) 0.0478(7) Uani 1 1 d . . . H11A H 0.0451 0.3688 0.9529 0.072 Uiso 1 1 calc . . . H11B H 0.0020 0.4223 1.0184 0.072 Uiso 1 1 calc . . . H11C H 0.0549 0.3524 1.0567 0.072 Uiso 1 1 calc . . . C12 C 0.2403(3) 0.44761(17) 1.1242(2) 0.0587(9) Uani 1 1 d . . . H12A H 0.2293 0.4174 1.1721 0.088 Uiso 1 1 calc . . . H12B H 0.1755 0.4837 1.1222 0.088 Uiso 1 1 calc . . . H12C H 0.3342 0.4646 1.1360 0.088 Uiso 1 1 calc . . . C13 C -0.1008(2) 0.54520(12) 0.63756(15) 0.0264(5) Uani 1 1 d . . . C14 C -0.2038(2) 0.49700(12) 0.61773(15) 0.0285(5) Uani 1 1 d . . . C15 C -0.3404(3) 0.51704(13) 0.59491(17) 0.0379(6) Uani 1 1 d . . . H15 H -0.4109 0.4853 0.5822 0.046 Uiso 1 1 calc R . . C16 C -0.3748(3) 0.58219(14) 0.59047(18) 0.0418(6) Uani 1 1 d . . . H16 H -0.4684 0.5949 0.5760 0.050 Uiso 1 1 calc R . . C17 C -0.2729(3) 0.62893(13) 0.60717(17) 0.0367(6) Uani 1 1 d . . . H17 H -0.2973 0.6737 0.6025 0.044 Uiso 1 1 calc R . . C18 C -0.1353(2) 0.61161(11) 0.63064(15) 0.0282(5) Uani 1 1 d . . . C19 C -0.0230(3) 0.66241(11) 0.65016(17) 0.0330(6) Uani 1 1 d . . . H19 H 0.0622 0.6422 0.6371 0.040 Uiso 1 1 calc R . . C20 C -0.0530(3) 0.72303(14) 0.5911(2) 0.0515(8) Uani 1 1 d . . . H20A H -0.0727 0.7101 0.5279 0.077 Uiso 1 1 calc . . . H20B H 0.0269 0.7519 0.6025 0.077 Uiso 1 1 calc . . . H20C H -0.1324 0.7459 0.6053 0.077 Uiso 1 1 calc . . . C21 C 0.0065(3) 0.68077(14) 0.7495(2) 0.0474(7) Uani 1 1 d . . . H21A H -0.0754 0.7005 0.7649 0.071 Uiso 1 1 calc . . . H21B H 0.0825 0.7119 0.7614 0.071 Uiso 1 1 calc . . . H21C H 0.0314 0.6416 0.7859 0.071 Uiso 1 1 calc . . . C22 C -0.1688(3) 0.42518(12) 0.61609(16) 0.0307(5) Uani 1 1 d . . . H22 H -0.0701 0.4206 0.6454 0.037 Uiso 1 1 calc R . . C23 C -0.2506(4) 0.38300(15) 0.6685(2) 0.0607(9) Uani 1 1 d . . . H23A H -0.2419 0.4004 0.7293 0.091 Uiso 1 1 calc . . . H23B H -0.2151 0.3384 0.6716 0.091 Uiso 1 1 calc . . . H23C H -0.3473 0.3830 0.6385 0.091 Uiso 1 1 calc . . . C24 C -0.1833(3) 0.40083(14) 0.51987(18) 0.0418(6) Uani 1 1 d . . . H24A H -0.2783 0.4063 0.4880 0.063 Uiso 1 1 calc . . . H24B H -0.1584 0.3547 0.5205 0.063 Uiso 1 1 calc . . . H24C H -0.1223 0.4258 0.4894 0.063 Uiso 1 1 calc . . . C25 C 0.3297(3) 0.57738(12) 0.73553(19) 0.0388(6) Uani 1 1 d . . . H25A H 0.2711 0.6153 0.7387 0.058 Uiso 1 1 calc . . . H25B H 0.3064 0.5582 0.6755 0.058 Uiso 1 1 calc . . . H25C H 0.4260 0.5909 0.7479 0.058 Uiso 1 1 calc . . . C26 C 0.3408(3) 0.55842(13) 0.89284(18) 0.0389(6) Uani 1 1 d . . . H26A H 0.4348 0.5752 0.9039 0.058 Uiso 1 1 calc . . . H26B H 0.3324 0.5257 0.9382 0.058 Uiso 1 1 calc . . . H26C H 0.2770 0.5942 0.8961 0.058 Uiso 1 1 calc . . . C27 C 0.2163(3) 0.41942(14) 0.61301(17) 0.0400(6) Uani 1 1 d . . . H27A H 0.2819 0.3902 0.5929 0.060 Uiso 1 1 calc . . . H27B H 0.2394 0.4646 0.6019 0.060 Uiso 1 1 calc . . . H27C H 0.1235 0.4098 0.5799 0.060 Uiso 1 1 calc . . . C28 C 0.1867(3) 0.34174(12) 0.72608(18) 0.0394(6) Uani 1 1 d . . . H28A H 0.0945 0.3322 0.6919 0.059 Uiso 1 1 calc . . . H28B H 0.1888 0.3353 0.7901 0.059 Uiso 1 1 calc . . . H28C H 0.2529 0.3125 0.7068 0.059 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02264(9) 0.02386(9) 0.02500(9) -0.00080(6) 0.00616(6) 0.00105(6) Sn2 0.02366(9) 0.03006(10) 0.03358(10) 0.00680(7) 0.01004(7) 0.00511(6) N1 0.0256(10) 0.0228(10) 0.0323(10) 0.0015(8) 0.0027(8) -0.0003(8) N2 0.0322(11) 0.0221(10) 0.0251(10) 0.0000(8) 0.0050(8) 0.0054(8) O1 0.0357(9) 0.0331(9) 0.0300(9) 0.0073(7) 0.0130(7) 0.0100(8) O2 0.0246(8) 0.0297(9) 0.0325(9) 0.0072(7) 0.0059(7) 0.0059(7) C1 0.0243(11) 0.0249(12) 0.0252(11) 0.0009(9) 0.0020(9) -0.0027(9) C2 0.0262(12) 0.0295(13) 0.0322(13) -0.0016(10) 0.0065(10) -0.0057(10) C3 0.0404(15) 0.0448(16) 0.0369(14) 0.0077(12) 0.0147(12) -0.0052(12) C4 0.0469(16) 0.0445(16) 0.0418(15) 0.0170(13) 0.0099(13) -0.0003(13) C5 0.0343(14) 0.0291(13) 0.0433(15) 0.0081(11) 0.0077(11) 0.0034(11) C6 0.0257(12) 0.0269(12) 0.0285(12) -0.0002(10) 0.0027(9) -0.0004(10) C7 0.0310(13) 0.0297(13) 0.0302(12) 0.0039(10) 0.0059(10) 0.0077(10) C8 0.0349(14) 0.0555(18) 0.0408(15) 0.0036(13) 0.0144(12) -0.0008(13) C9 0.067(2) 0.0353(15) 0.0506(17) 0.0012(13) 0.0220(15) 0.0163(14) C10 0.0297(13) 0.0341(14) 0.0402(14) -0.0014(11) 0.0149(11) -0.0025(11) C11 0.0337(15) 0.0512(18) 0.0573(18) -0.0082(14) 0.0064(13) -0.0006(13) C12 0.0440(18) 0.065(2) 0.067(2) -0.0305(17) 0.0093(15) -0.0002(15) C13 0.0250(12) 0.0325(13) 0.0223(11) 0.0024(10) 0.0067(9) 0.0061(10) C14 0.0287(12) 0.0339(13) 0.0228(11) 0.0013(10) 0.0051(9) 0.0029(10) C15 0.0297(14) 0.0453(16) 0.0375(14) -0.0016(12) 0.0037(11) -0.0028(12) C16 0.0270(13) 0.0500(17) 0.0467(16) 0.0009(13) 0.0037(11) 0.0120(12) C17 0.0363(14) 0.0350(14) 0.0397(14) 0.0042(11) 0.0098(11) 0.0132(11) C18 0.0306(13) 0.0293(13) 0.0256(12) 0.0002(10) 0.0076(10) 0.0061(10) C19 0.0359(14) 0.0250(13) 0.0405(14) 0.0012(10) 0.0134(11) 0.0047(10) C20 0.0552(19) 0.0334(15) 0.069(2) 0.0128(14) 0.0198(16) 0.0044(13) C21 0.0497(17) 0.0412(16) 0.0514(17) -0.0093(13) 0.0103(14) -0.0051(13) C22 0.0314(13) 0.0294(13) 0.0304(13) -0.0022(10) 0.0040(10) -0.0019(10) C23 0.084(2) 0.0391(17) 0.071(2) 0.0099(15) 0.0448(19) 0.0019(16) C24 0.0443(16) 0.0422(16) 0.0370(14) -0.0073(12) 0.0037(12) 0.0025(13) C25 0.0343(14) 0.0297(14) 0.0523(16) 0.0113(12) 0.0084(12) -0.0022(11) C26 0.0371(15) 0.0342(14) 0.0423(15) -0.0095(12) 0.0003(12) -0.0071(11) C27 0.0441(15) 0.0477(16) 0.0295(13) -0.0035(12) 0.0103(11) 0.0113(13) C28 0.0440(15) 0.0251(13) 0.0479(16) -0.0042(11) 0.0067(12) 0.0020(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O2 2.0590(15) . ? Sn1 N1 2.2356(19) . ? Sn1 N2 2.2447(18) . ? Sn2 O1 2.0592(15) . ? Sn2 N2 2.2264(19) . ? Sn2 N1 2.2272(19) . ? N1 C26 1.477(3) . ? N1 C25 1.482(3) . ? N2 C28 1.477(3) . ? N2 C27 1.483(3) . ? O1 C1 1.350(3) . ? O2 C13 1.363(3) . ? C1 C2 1.416(3) . ? C1 C6 1.417(3) . ? C2 C3 1.390(3) . ? C2 C10 1.521(3) . ? C3 C4 1.384(4) . ? C3 H3 0.9500 . ? C4 C5 1.376(4) . ? C4 H4 0.9500 . ? C5 C6 1.392(3) . ? C5 H5 0.9500 . ? C6 C7 1.515(3) . ? C7 C9 1.527(4) . ? C7 C8 1.529(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.522(4) . ? C10 C12 1.526(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.406(3) . ? C13 C14 1.415(3) . ? C14 C15 1.397(3) . ? C14 C22 1.518(3) . ? C15 C16 1.381(4) . ? C15 H15 0.9500 . ? C16 C17 1.384(4) . ? C16 H16 0.9500 . ? C17 C18 1.391(3) . ? C17 H17 0.9500 . ? C18 C19 1.515(3) . ? C19 C21 1.529(4) . ? C19 C20 1.531(4) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.520(4) . ? C22 C24 1.528(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sn1 N1 93.07(7) . . ? O2 Sn1 N2 91.10(6) . . ? N1 Sn1 N2 79.39(7) . . ? O1 Sn2 N2 85.60(7) . . ? O1 Sn2 N1 86.28(7) . . ? N2 Sn2 N1 79.96(7) . . ? C26 N1 C25 108.90(19) . . ? C26 N1 Sn2 115.04(15) . . ? C25 N1 Sn2 108.54(15) . . ? C26 N1 Sn1 111.35(15) . . ? C25 N1 Sn1 116.84(15) . . ? Sn2 N1 Sn1 95.87(7) . . ? C28 N2 C27 109.0(2) . . ? C28 N2 Sn2 113.86(15) . . ? C27 N2 Sn2 109.34(15) . . ? C28 N2 Sn1 110.97(15) . . ? C27 N2 Sn1 117.63(14) . . ? Sn2 N2 Sn1 95.63(7) . . ? C1 O1 Sn2 142.22(14) . . ? C13 O2 Sn1 119.95(13) . . ? O1 C1 C2 117.2(2) . . ? O1 C1 C6 123.0(2) . . ? C2 C1 C6 119.9(2) . . ? C3 C2 C1 118.8(2) . . ? C3 C2 C10 119.9(2) . . ? C1 C2 C10 121.2(2) . . ? C4 C3 C2 121.5(2) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 122.0(2) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 118.4(2) . . ? C5 C6 C7 119.6(2) . . ? C1 C6 C7 121.8(2) . . ? C6 C7 C9 114.7(2) . . ? C6 C7 C8 110.2(2) . . ? C9 C7 C8 110.2(2) . . ? C6 C7 H7 107.1 . . ? C9 C7 H7 107.1 . . ? C8 C7 H7 107.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C11 111.9(2) . . ? C2 C10 C12 112.7(2) . . ? C11 C10 C12 110.4(2) . . ? C2 C10 H10 107.2 . . ? C11 C10 H10 107.2 . . ? C12 C10 H10 107.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 C18 118.6(2) . . ? O2 C13 C14 120.8(2) . . ? C18 C13 C14 120.5(2) . . ? C15 C14 C13 118.4(2) . . ? C15 C14 C22 119.9(2) . . ? C13 C14 C22 121.7(2) . . ? C16 C15 C14 121.2(3) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 119.9(2) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 121.2(2) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C13 118.7(2) . . ? C17 C18 C19 121.6(2) . . ? C13 C18 C19 119.7(2) . . ? C18 C19 C21 110.7(2) . . ? C18 C19 C20 113.3(2) . . ? C21 C19 C20 110.9(2) . . ? C18 C19 H19 107.2 . . ? C21 C19 H19 107.2 . . ? C20 C19 H19 107.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 C23 113.4(2) . . ? C14 C22 C24 110.9(2) . . ? C23 C22 C24 111.0(2) . . ? C14 C22 H22 107.0 . . ? C23 C22 H22 107.0 . . ? C24 C22 H22 107.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 H26A 109.5 . . ? N1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C28 H28A 109.5 . . ? N2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.646 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.069 #===END data_mar312_0m _database_code_depnum_ccdc_archive 'CCDC 843202' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H54 N2 O2 Sn2' _chemical_formula_sum 'C32 H54 N2 O2 Sn2' _chemical_formula_weight 736.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0543(15) _cell_length_b 12.3130(12) _cell_length_c 18.4523(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.9500(10) _cell_angle_gamma 90.00 _cell_volume 3358.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 9947 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.11 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.412 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.155 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.791 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27315 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.19 _reflns_number_total 7634 _reflns_number_gt 7052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+1.6997P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7634 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.204483(8) 0.178058(10) 0.246881(6) 0.02539(4) Uani 1 1 d . . . Sn2 Sn 0.102214(8) 0.042204(10) 0.091953(6) 0.02384(4) Uani 1 1 d . . . N1 N 0.13778(10) 0.01583(12) 0.21651(8) 0.0256(3) Uani 1 1 d . . . N2 N 0.22251(10) 0.15440(12) 0.12904(8) 0.0257(3) Uani 1 1 d . . . O1 O 0.33093(8) 0.12367(10) 0.29930(7) 0.0273(3) Uani 1 1 d . . . O2 O 0.17478(8) -0.08960(10) 0.05992(6) 0.0253(2) Uani 1 1 d . . . C1 C 0.37714(12) 0.16986(15) 0.36332(10) 0.0261(4) Uani 1 1 d . . . C2 C 0.43686(12) 0.25866(15) 0.36019(10) 0.0287(4) Uani 1 1 d . . . C3 C 0.47098(13) 0.31398(16) 0.42567(11) 0.0334(4) Uani 1 1 d . . . H3 H 0.5063 0.3755 0.4238 0.040 Uiso 1 1 calc R . . C4 C 0.45393(13) 0.28026(18) 0.49303(11) 0.0348(4) Uani 1 1 d . . . H4 H 0.4737 0.3213 0.5353 0.042 Uiso 1 1 calc R . . C5 C 0.40726(13) 0.18496(17) 0.49653(11) 0.0320(4) Uani 1 1 d . . . H5 H 0.4001 0.1591 0.5424 0.038 Uiso 1 1 calc R . . C6 C 0.37034(12) 0.12576(15) 0.43351(10) 0.0277(4) Uani 1 1 d . . . C7 C 0.32695(13) 0.01440(17) 0.44282(11) 0.0328(4) Uani 1 1 d . . . C8 C 0.22323(14) 0.02386(18) 0.42322(12) 0.0382(5) Uani 1 1 d . . . H8A H 0.2058 0.0525 0.3742 0.057 Uiso 1 1 calc R . . H8B H 0.2025 0.0716 0.4576 0.057 Uiso 1 1 calc R . . H8C H 0.1967 -0.0466 0.4256 0.057 Uiso 1 1 calc R . . C9 C 0.36451(15) -0.07159(17) 0.39597(12) 0.0380(4) Uani 1 1 d . . . H9A H 0.3586 -0.0459 0.3462 0.057 Uiso 1 1 calc R . . H9B H 0.3312 -0.1380 0.3963 0.057 Uiso 1 1 calc R . . H9C H 0.4272 -0.0845 0.4162 0.057 Uiso 1 1 calc R . . C10 C 0.35087(18) -0.0277(2) 0.52271(12) 0.0487(6) Uani 1 1 d . . . H10A H 0.3271 -0.0996 0.5251 0.073 Uiso 1 1 calc R . . H10B H 0.3250 0.0196 0.5545 0.073 Uiso 1 1 calc R . . H10C H 0.4154 -0.0292 0.5383 0.073 Uiso 1 1 calc R . . C11 C 0.47158(14) 0.28984(18) 0.28947(11) 0.0353(4) Uani 1 1 d . . . C12 C 0.54937(17) 0.3733(2) 0.30534(13) 0.0551(7) Uani 1 1 d . . . H12A H 0.5714 0.3876 0.2608 0.083 Uiso 1 1 calc R . . H12B H 0.5975 0.3446 0.3420 0.083 Uiso 1 1 calc R . . H12C H 0.5275 0.4395 0.3231 0.083 Uiso 1 1 calc R . . C13 C 0.39787(15) 0.34232(18) 0.23148(11) 0.0397(5) Uani 1 1 d . . . H13A H 0.3484 0.2925 0.2181 0.059 Uiso 1 1 calc R . . H13B H 0.4222 0.3601 0.1885 0.059 Uiso 1 1 calc R . . H13C H 0.3767 0.4073 0.2514 0.059 Uiso 1 1 calc R . . C14 C 0.51072(16) 0.1881(2) 0.25921(13) 0.0454(5) Uani 1 1 d . . . H14A H 0.4653 0.1325 0.2504 0.068 Uiso 1 1 calc R . . H14B H 0.5617 0.1626 0.2945 0.068 Uiso 1 1 calc R . . H14C H 0.5297 0.2055 0.2138 0.068 Uiso 1 1 calc R . . C15 C 0.14160(11) -0.15406(14) 0.00073(10) 0.0246(3) Uani 1 1 d . . . C16 C 0.09223(12) -0.25005(14) 0.00993(10) 0.0269(4) Uani 1 1 d . . . C17 C 0.04621(13) -0.30211(16) -0.05361(12) 0.0336(4) Uani 1 1 d . . . H17 H 0.0099 -0.3617 -0.0484 0.040 Uiso 1 1 calc R . . C18 C 0.05265(14) -0.26842(17) -0.12352(11) 0.0365(5) Uani 1 1 d . . . H18 H 0.0170 -0.3000 -0.1648 0.044 Uiso 1 1 calc R . . C19 C 0.11312(14) -0.18674(16) -0.13118(11) 0.0329(4) Uani 1 1 d . . . H19 H 0.1228 -0.1695 -0.1781 0.039 Uiso 1 1 calc R . . C20 C 0.16004(12) -0.12932(15) -0.07076(10) 0.0270(4) Uani 1 1 d . . . C21 C 0.23332(14) -0.04759(16) -0.08247(11) 0.0318(4) Uani 1 1 d . . . C22 C 0.20430(15) 0.06988(17) -0.07172(12) 0.0373(4) Uani 1 1 d . . . H22A H 0.1512 0.0866 -0.1077 0.056 Uiso 1 1 calc R . . H22B H 0.2523 0.1184 -0.0777 0.056 Uiso 1 1 calc R . . H22C H 0.1913 0.0781 -0.0231 0.056 Uiso 1 1 calc R . . C23 C 0.32246(13) -0.07670(18) -0.02972(12) 0.0378(4) Uani 1 1 d . . . H23A H 0.3121 -0.0800 0.0200 0.057 Uiso 1 1 calc R . . H23B H 0.3671 -0.0222 -0.0331 0.057 Uiso 1 1 calc R . . H23C H 0.3436 -0.1460 -0.0433 0.057 Uiso 1 1 calc R . . C24 C 0.25410(19) -0.0535(2) -0.16117(13) 0.0531(6) Uani 1 1 d . . . H24A H 0.2693 -0.1268 -0.1717 0.080 Uiso 1 1 calc R . . H24B H 0.3041 -0.0065 -0.1645 0.080 Uiso 1 1 calc R . . H24C H 0.2018 -0.0308 -0.1962 0.080 Uiso 1 1 calc R . . C25 C 0.09042(14) -0.30008(15) 0.08591(11) 0.0316(4) Uani 1 1 d . . . C26 C 0.02639(14) -0.23513(17) 0.12558(12) 0.0369(4) Uani 1 1 d . . . H26A H 0.0300 -0.2631 0.1746 0.055 Uiso 1 1 calc R . . H26B H -0.0346 -0.2418 0.0987 0.055 Uiso 1 1 calc R . . H26C H 0.0438 -0.1600 0.1281 0.055 Uiso 1 1 calc R . . C27 C 0.18726(14) -0.30784(17) 0.13058(11) 0.0362(4) Uani 1 1 d . . . H27A H 0.1855 -0.3316 0.1798 0.054 Uiso 1 1 calc R . . H27B H 0.2156 -0.2378 0.1323 0.054 Uiso 1 1 calc R . . H27C H 0.2212 -0.3590 0.1075 0.054 Uiso 1 1 calc R . . C28 C 0.05433(17) -0.41738(17) 0.08016(13) 0.0461(5) Uani 1 1 d . . . H28A H 0.0881 -0.4600 0.0513 0.069 Uiso 1 1 calc R . . H28B H -0.0084 -0.4172 0.0569 0.069 Uiso 1 1 calc R . . H28C H 0.0607 -0.4481 0.1287 0.069 Uiso 1 1 calc R . . C29 C 0.19483(13) -0.08046(16) 0.24053(10) 0.0311(4) Uani 1 1 d . . . H29A H 0.2088 -0.0830 0.2935 0.047 Uiso 1 1 calc R . . H29B H 0.2499 -0.0756 0.2217 0.047 Uiso 1 1 calc R . . H29C H 0.1627 -0.1451 0.2220 0.047 Uiso 1 1 calc R . . C30 C 0.05363(12) 0.00910(16) 0.24716(10) 0.0303(4) Uani 1 1 d . . . H30A H 0.0186 -0.0523 0.2262 0.045 Uiso 1 1 calc R . . H30B H 0.0189 0.0743 0.2353 0.045 Uiso 1 1 calc R . . H30C H 0.0689 0.0010 0.2998 0.045 Uiso 1 1 calc R . . C31 C 0.20749(14) 0.25817(16) 0.08742(11) 0.0339(4) Uani 1 1 d . . . H31A H 0.2534 0.3095 0.1081 0.051 Uiso 1 1 calc R . . H31B H 0.1490 0.2867 0.0907 0.051 Uiso 1 1 calc R . . H31C H 0.2103 0.2454 0.0366 0.051 Uiso 1 1 calc R . . C32 C 0.31069(12) 0.10682(16) 0.12142(11) 0.0318(4) Uani 1 1 d . . . H32A H 0.3121 0.0965 0.0701 0.048 Uiso 1 1 calc R . . H32B H 0.3185 0.0381 0.1464 0.048 Uiso 1 1 calc R . . H32C H 0.3586 0.1550 0.1429 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02637(7) 0.02534(7) 0.02442(7) -0.00483(4) 0.00471(5) -0.00197(4) Sn2 0.02325(7) 0.02557(7) 0.02175(7) -0.00237(4) 0.00189(5) -0.00105(4) N1 0.0240(7) 0.0285(7) 0.0246(7) -0.0025(6) 0.0056(6) -0.0027(6) N2 0.0268(7) 0.0250(7) 0.0248(7) 0.0005(6) 0.0036(6) -0.0006(6) O1 0.0265(6) 0.0314(7) 0.0229(6) -0.0028(5) 0.0017(5) -0.0049(5) O2 0.0277(6) 0.0258(6) 0.0219(6) -0.0035(5) 0.0036(5) -0.0017(5) C1 0.0232(8) 0.0313(9) 0.0232(8) -0.0038(7) 0.0030(7) -0.0013(7) C2 0.0263(9) 0.0337(10) 0.0257(9) -0.0008(7) 0.0035(7) -0.0038(7) C3 0.0285(10) 0.0363(10) 0.0341(10) -0.0054(8) 0.0022(8) -0.0094(8) C4 0.0306(10) 0.0460(11) 0.0262(9) -0.0113(8) 0.0013(7) -0.0050(9) C5 0.0268(9) 0.0453(11) 0.0240(9) -0.0014(8) 0.0051(7) -0.0006(8) C6 0.0230(8) 0.0334(10) 0.0266(9) 0.0001(7) 0.0045(7) -0.0017(7) C7 0.0341(10) 0.0356(10) 0.0290(10) 0.0004(8) 0.0070(8) -0.0061(8) C8 0.0340(11) 0.0453(12) 0.0375(11) -0.0040(9) 0.0119(9) -0.0119(9) C9 0.0384(11) 0.0350(10) 0.0393(11) 0.0025(9) 0.0040(9) 0.0009(9) C10 0.0610(15) 0.0521(14) 0.0320(11) 0.0081(10) 0.0062(10) -0.0140(11) C11 0.0339(10) 0.0436(11) 0.0292(10) -0.0030(8) 0.0078(8) -0.0149(9) C12 0.0523(14) 0.0735(18) 0.0400(12) -0.0006(12) 0.0103(10) -0.0363(13) C13 0.0497(13) 0.0378(11) 0.0309(10) 0.0011(8) 0.0063(9) -0.0097(9) C14 0.0370(12) 0.0607(15) 0.0414(12) -0.0028(10) 0.0146(9) -0.0022(10) C15 0.0222(8) 0.0269(8) 0.0241(8) -0.0039(7) 0.0029(6) 0.0029(7) C16 0.0269(9) 0.0242(8) 0.0299(9) -0.0035(7) 0.0062(7) 0.0015(7) C17 0.0315(10) 0.0262(9) 0.0411(11) -0.0100(8) 0.0022(8) -0.0005(8) C18 0.0372(11) 0.0358(10) 0.0323(10) -0.0154(8) -0.0045(8) 0.0039(8) C19 0.0353(10) 0.0386(10) 0.0238(9) -0.0051(8) 0.0030(7) 0.0080(8) C20 0.0262(9) 0.0296(9) 0.0249(9) -0.0029(7) 0.0038(7) 0.0039(7) C21 0.0332(10) 0.0384(11) 0.0252(9) 0.0003(8) 0.0092(8) -0.0004(8) C22 0.0414(11) 0.0355(10) 0.0346(11) 0.0063(8) 0.0064(9) 0.0000(9) C23 0.0275(10) 0.0417(11) 0.0453(12) -0.0010(9) 0.0099(8) 0.0013(8) C24 0.0618(16) 0.0692(17) 0.0336(12) -0.0025(11) 0.0229(11) -0.0114(13) C25 0.0368(10) 0.0243(9) 0.0356(10) -0.0026(7) 0.0119(8) -0.0036(8) C26 0.0374(11) 0.0363(11) 0.0401(11) -0.0056(9) 0.0151(9) -0.0036(9) C27 0.0426(12) 0.0328(10) 0.0342(10) 0.0052(8) 0.0095(9) 0.0076(8) C28 0.0633(15) 0.0310(11) 0.0483(13) -0.0060(9) 0.0217(11) -0.0111(10) C29 0.0321(10) 0.0301(10) 0.0293(9) -0.0033(7) 0.0017(7) 0.0010(8) C30 0.0272(9) 0.0348(10) 0.0299(9) -0.0026(8) 0.0083(7) -0.0040(8) C31 0.0364(10) 0.0295(9) 0.0342(10) 0.0052(8) 0.0021(8) -0.0037(8) C32 0.0280(9) 0.0373(10) 0.0300(9) -0.0033(8) 0.0055(7) -0.0003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.0757(13) . ? Sn1 N1 2.2580(15) . ? Sn1 N2 2.2607(15) . ? Sn2 O2 2.1028(12) . ? Sn2 N2 2.2772(15) . ? Sn2 N1 2.2819(15) . ? N1 C29 1.482(2) . ? N1 C30 1.485(2) . ? N2 C32 1.482(2) . ? N2 C31 1.486(2) . ? O1 C1 1.375(2) . ? O2 C15 1.366(2) . ? C1 C2 1.424(3) . ? C1 C6 1.426(3) . ? C2 C3 1.397(3) . ? C2 C11 1.544(3) . ? C3 C4 1.380(3) . ? C3 H3 0.9300 . ? C4 C5 1.375(3) . ? C4 H4 0.9300 . ? C5 C6 1.395(3) . ? C5 H5 0.9300 . ? C6 C7 1.542(3) . ? C7 C8 1.539(3) . ? C7 C10 1.539(3) . ? C7 C9 1.541(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C13 1.531(3) . ? C11 C14 1.534(3) . ? C11 C12 1.544(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.423(2) . ? C15 C20 1.432(3) . ? C16 C17 1.399(3) . ? C16 C25 1.536(3) . ? C17 C18 1.376(3) . ? C17 H17 0.9300 . ? C18 C19 1.382(3) . ? C18 H18 0.9300 . ? C19 C20 1.394(3) . ? C19 H19 0.9300 . ? C20 C21 1.538(3) . ? C21 C22 1.535(3) . ? C21 C23 1.543(3) . ? C21 C24 1.544(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C27 1.535(3) . ? C25 C28 1.540(3) . ? C25 C26 1.540(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 N1 98.95(5) . . ? O1 Sn1 N2 98.03(5) . . ? N1 Sn1 N2 77.07(5) . . ? O2 Sn2 N2 97.28(5) . . ? O2 Sn2 N1 97.95(5) . . ? N2 Sn2 N1 76.26(5) . . ? C29 N1 C30 109.24(15) . . ? C29 N1 Sn1 115.37(11) . . ? C30 N1 Sn1 109.04(11) . . ? C29 N1 Sn2 115.27(11) . . ? C30 N1 Sn2 109.74(11) . . ? Sn1 N1 Sn2 97.60(6) . . ? C32 N2 C31 110.00(15) . . ? C32 N2 Sn1 114.56(11) . . ? C31 N2 Sn1 110.61(11) . . ? C32 N2 Sn2 114.03(11) . . ? C31 N2 Sn2 109.40(11) . . ? Sn1 N2 Sn2 97.66(6) . . ? C1 O1 Sn1 122.44(11) . . ? C15 O2 Sn2 122.87(10) . . ? O1 C1 C2 120.21(16) . . ? O1 C1 C6 120.73(16) . . ? C2 C1 C6 118.95(16) . . ? C3 C2 C1 118.08(17) . . ? C3 C2 C11 118.81(17) . . ? C1 C2 C11 122.90(16) . . ? C4 C3 C2 122.10(18) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C5 C4 C3 118.89(18) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 122.18(18) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 118.17(17) . . ? C5 C6 C7 118.80(17) . . ? C1 C6 C7 123.00(16) . . ? C8 C7 C10 107.03(17) . . ? C8 C7 C9 112.60(17) . . ? C10 C7 C9 105.20(18) . . ? C8 C7 C6 109.81(17) . . ? C10 C7 C6 112.26(16) . . ? C9 C7 C6 109.88(16) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C14 111.59(17) . . ? C13 C11 C12 105.95(19) . . ? C14 C11 C12 106.42(19) . . ? C13 C11 C2 112.28(17) . . ? C14 C11 C2 108.64(17) . . ? C12 C11 C2 111.82(17) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 120.48(16) . . ? O2 C15 C20 120.51(16) . . ? C16 C15 C20 118.92(16) . . ? C17 C16 C15 117.86(17) . . ? C17 C16 C25 119.30(17) . . ? C15 C16 C25 122.81(16) . . ? C18 C17 C16 122.40(19) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C17 C18 C19 118.71(18) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C18 C19 C20 122.08(19) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C20 C15 118.14(17) . . ? C19 C20 C21 119.17(17) . . ? C15 C20 C21 122.57(16) . . ? C22 C21 C20 111.66(16) . . ? C22 C21 C23 111.85(17) . . ? C20 C21 C23 108.69(16) . . ? C22 C21 C24 106.21(18) . . ? C20 C21 C24 112.34(17) . . ? C23 C21 C24 105.96(18) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C16 109.58(16) . . ? C27 C25 C28 105.38(17) . . ? C16 C25 C28 112.36(16) . . ? C27 C25 C26 113.16(17) . . ? C16 C25 C26 110.29(16) . . ? C28 C25 C26 105.98(17) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 H31A 109.5 . . ? N2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.574 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.062 #===END data_11my231_0m _database_code_depnum_ccdc_archive 'CCDC 843204' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H70 O10 Sn5' _chemical_formula_sum 'C70 H70 O10 Sn5' _chemical_formula_weight 1664.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.166(2) _cell_length_b 12.382(2) _cell_length_c 26.605(5) _cell_angle_alpha 99.731(2) _cell_angle_beta 92.217(2) _cell_angle_gamma 111.074(2) _cell_volume 3363.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 9995 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.34 _exptl_crystal_description Prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 1.887 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.420 _exptl_absorpt_correction_T_max 0.660 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24912 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12167 _reflns_number_gt 10471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some of the phenyl rings have non-standard geometry, so the restraint ofAFIX 66 was added to C64-C69 and C1- C6. In addition EADP was used for these rings to constrain the ADPs. Some residual disorder is present for which applying restraints/constraint did not fix. This can account for any residual density SQUEEZE was used to remove a disordered toluene that was in the lattice ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+7.8821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12167 _refine_ls_number_parameters 716 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.16708(3) 0.08203(3) 0.488215(11) 0.03158(8) Uani 1 1 d . . . Sn2 Sn 0.13886(3) 0.06648(3) 0.349017(11) 0.02962(8) Uani 1 1 d . . . Sn3 Sn 0.44991(3) 0.14838(3) 0.296940(11) 0.03010(8) Uani 1 1 d . . . Sn4 Sn 0.42451(3) 0.09199(3) 0.157125(11) 0.03039(8) Uani 1 1 d . . . Sn5 Sn 0.62507(3) 0.09070(3) 0.053171(12) 0.04004(9) Uani 1 1 d . . . O1 O 0.0120(3) -0.0852(3) 0.46778(11) 0.0339(7) Uani 1 1 d . . . O2 O 0.2503(3) 0.0368(3) 0.40933(11) 0.0313(6) Uani 1 1 d . . . O3 O 0.0993(3) 0.1495(3) 0.42975(11) 0.0343(7) Uani 1 1 d . . . O4 O 0.2948(3) 0.2214(3) 0.34141(11) 0.0343(7) Uani 1 1 d . . . O5 O 0.2612(3) 0.0141(3) 0.28216(11) 0.0319(6) Uani 1 1 d . . . O6 O 0.4304(3) 0.2312(2) 0.23398(11) 0.0321(6) Uani 1 1 d . . . O7 O 0.5049(3) 0.0562(3) 0.22393(10) 0.0334(7) Uani 1 1 d . . . O8 O 0.5199(3) -0.0194(3) 0.10207(11) 0.0354(7) Uani 1 1 d . . . O9 O 0.5994(3) 0.2037(3) 0.12980(11) 0.0380(7) Uani 1 1 d . . . O10 O 0.4473(3) 0.0766(3) 0.01517(12) 0.0412(8) Uani 1 1 d . . . C1 C -0.0068(3) -0.1734(2) 0.42519(10) 0.0380(11) Uani 1 1 d G . . C2 C -0.0982(3) -0.1850(3) 0.38562(13) 0.0553(14) Uani 1 1 d G . . H2 H -0.1423 -0.1318 0.3880 0.066 Uiso 1 1 calc R . . C3 C -0.1252(3) -0.2745(3) 0.34262(11) 0.0673(17) Uani 1 1 d G . . H3 H -0.1877 -0.2824 0.3156 0.081 Uiso 1 1 calc R . . C4 C -0.0607(4) -0.3524(3) 0.33919(12) 0.0677(17) Uani 1 1 d G . . H4 H -0.0791 -0.4135 0.3098 0.081 Uiso 1 1 calc R . . C5 C 0.0308(3) -0.3408(3) 0.37876(14) 0.0577(15) Uani 1 1 d G . . H5 H 0.0749 -0.3940 0.3764 0.069 Uiso 1 1 calc R . . C6 C 0.0577(3) -0.2513(3) 0.42176(11) 0.0478(12) Uani 1 1 d G . . C7 C 0.1612(6) -0.2341(5) 0.4621(2) 0.0561(14) Uani 1 1 d . . . H7A H 0.1846 -0.3039 0.4575 0.084 Uiso 1 1 calc R . . H7B H 0.1306 -0.2224 0.4959 0.084 Uiso 1 1 calc R . . H7C H 0.2369 -0.1645 0.4597 0.084 Uiso 1 1 calc R . . C8 C 0.3443(4) -0.0101(4) 0.40116(16) 0.0320(9) Uani 1 1 d . . . C9 C 0.3172(5) -0.1128(4) 0.36504(18) 0.0401(11) Uani 1 1 d . . . H9 H 0.2340 -0.1505 0.3463 0.048 Uiso 1 1 calc R . . C10 C 0.4106(6) -0.1610(5) 0.3561(2) 0.0575(15) Uani 1 1 d . . . H10 H 0.3914 -0.2315 0.3313 0.069 Uiso 1 1 calc R . . C11 C 0.5316(6) -0.1068(6) 0.3831(2) 0.0648(17) Uani 1 1 d . . . H11 H 0.5960 -0.1394 0.3771 0.078 Uiso 1 1 calc R . . C12 C 0.5577(5) -0.0059(6) 0.4187(2) 0.0538(14) Uani 1 1 d . . . H12 H 0.6411 0.0307 0.4372 0.065 Uiso 1 1 calc R . . C13 C 0.4669(4) 0.0455(4) 0.42885(18) 0.0400(11) Uani 1 1 d . . . C14 C 0.5044(5) 0.1573(5) 0.4689(2) 0.0513(13) Uani 1 1 d . . . H14A H 0.4975 0.1374 0.5031 0.077 Uiso 1 1 calc R . . H14B H 0.4466 0.1987 0.4632 0.077 Uiso 1 1 calc R . . H14C H 0.5936 0.2082 0.4665 0.077 Uiso 1 1 calc R . . C15 C 0.0200(4) 0.2116(4) 0.42733(16) 0.0328(10) Uani 1 1 d . . . C16 C -0.1014(4) 0.1558(4) 0.39848(17) 0.0380(10) Uani 1 1 d . . . H16 H -0.1313 0.0739 0.3839 0.046 Uiso 1 1 calc R . . C17 C -0.1778(5) 0.2204(5) 0.39120(19) 0.0471(12) Uani 1 1 d . . . H17 H -0.2603 0.1823 0.3719 0.057 Uiso 1 1 calc R . . C18 C -0.1348(5) 0.3387(5) 0.4117(2) 0.0514(13) Uani 1 1 d . . . H18 H -0.1855 0.3834 0.4056 0.062 Uiso 1 1 calc R . . C19 C -0.0172(5) 0.3922(5) 0.44120(19) 0.0470(12) Uani 1 1 d . . . H19 H 0.0113 0.4740 0.4556 0.056 Uiso 1 1 calc R . . C20 C 0.0611(4) 0.3312(4) 0.45079(17) 0.0361(10) Uani 1 1 d . . . C21 C 0.1846(5) 0.3895(4) 0.48610(18) 0.0448(12) Uani 1 1 d . . . H21A H 0.2067 0.4751 0.4936 0.067 Uiso 1 1 calc R . . H21B H 0.2541 0.3718 0.4696 0.067 Uiso 1 1 calc R . . H21C H 0.1734 0.3597 0.5181 0.067 Uiso 1 1 calc R . . C22 C 0.3362(4) 0.3355(4) 0.36828(16) 0.0333(10) Uani 1 1 d . . . C23 C 0.4465(5) 0.3785(5) 0.40352(19) 0.0485(12) Uani 1 1 d . . . H23 H 0.4884 0.3275 0.4108 0.058 Uiso 1 1 calc R . . C24 C 0.4946(5) 0.4965(6) 0.4279(2) 0.0628(17) Uani 1 1 d . . . H24 H 0.5697 0.5259 0.4519 0.075 Uiso 1 1 calc R . . C25 C 0.4350(6) 0.5712(5) 0.4178(3) 0.0673(18) Uani 1 1 d . . . H25 H 0.4690 0.6521 0.4340 0.081 Uiso 1 1 calc R . . C26 C 0.3259(6) 0.5268(5) 0.3840(2) 0.0532(14) Uani 1 1 d . . . H26 H 0.2843 0.5786 0.3775 0.064 Uiso 1 1 calc R . . C27 C 0.2726(5) 0.4101(4) 0.35864(17) 0.0380(10) Uani 1 1 d . . . C28 C 0.1534(5) 0.3650(5) 0.3217(2) 0.0486(13) Uani 1 1 d . . . H28A H 0.0815 0.3127 0.3367 0.073 Uiso 1 1 calc R . . H28B H 0.1678 0.3211 0.2898 0.073 Uiso 1 1 calc R . . H28C H 0.1325 0.4316 0.3144 0.073 Uiso 1 1 calc R . . C29 C 0.1853(4) -0.0262(4) 0.23562(16) 0.0343(10) Uani 1 1 d . . . C30 C 0.1319(4) 0.0472(4) 0.21672(18) 0.0395(11) Uani 1 1 d . . . H30 H 0.1477 0.1237 0.2361 0.047 Uiso 1 1 calc R . . C31 C 0.0566(5) 0.0096(5) 0.1702(2) 0.0522(13) Uani 1 1 d . . . H31 H 0.0207 0.0600 0.1576 0.063 Uiso 1 1 calc R . . C32 C 0.0334(5) -0.1024(6) 0.1419(2) 0.0570(14) Uani 1 1 d . . . H32 H -0.0166 -0.1284 0.1094 0.068 Uiso 1 1 calc R . . C33 C 0.0832(5) -0.1753(5) 0.1612(2) 0.0511(13) Uani 1 1 d . . . H33 H 0.0661 -0.2521 0.1418 0.061 Uiso 1 1 calc R . . C34 C 0.1584(4) -0.1398(4) 0.20849(18) 0.0396(11) Uani 1 1 d . . . C35 C 0.2062(6) -0.2239(5) 0.2298(2) 0.0543(14) Uani 1 1 d . . . H35A H 0.2924 -0.1802 0.2483 0.081 Uiso 1 1 calc R . . H35B H 0.2105 -0.2841 0.2016 0.081 Uiso 1 1 calc R . . H35C H 0.1469 -0.2620 0.2533 0.081 Uiso 1 1 calc R . . C36 C 0.4028(5) 0.3304(4) 0.23282(18) 0.0393(11) Uani 1 1 d . . . C37 C 0.3038(5) 0.3251(5) 0.1985(2) 0.0515(13) Uani 1 1 d . . . H37 H 0.2530 0.2521 0.1768 0.062 Uiso 1 1 calc R . . C38 C 0.2781(7) 0.4260(7) 0.1956(3) 0.071(2) Uani 1 1 d . . . H38 H 0.2101 0.4221 0.1719 0.085 Uiso 1 1 calc R . . C39 C 0.3519(8) 0.5318(7) 0.2273(3) 0.081(2) Uani 1 1 d . . . H39 H 0.3339 0.6007 0.2260 0.097 Uiso 1 1 calc R . . C40 C 0.4504(8) 0.5370(5) 0.2605(3) 0.071(2) Uani 1 1 d . . . H40 H 0.4996 0.6105 0.2822 0.085 Uiso 1 1 calc R . . C41 C 0.4825(6) 0.4397(4) 0.2641(2) 0.0502(14) Uani 1 1 d . . . C42 C 0.5990(6) 0.4513(5) 0.2968(2) 0.0613(16) Uani 1 1 d . . . H42A H 0.6342 0.5299 0.3188 0.092 Uiso 1 1 calc R . . H42B H 0.6642 0.4406 0.2749 0.092 Uiso 1 1 calc R . . H42C H 0.5757 0.3911 0.3181 0.092 Uiso 1 1 calc R . . C43 C 0.6001(5) 0.0124(4) 0.23305(17) 0.0371(10) Uani 1 1 d . . . C44 C 0.5701(5) -0.1064(5) 0.22574(19) 0.0451(12) Uani 1 1 d . . . H44 H 0.4841 -0.1587 0.2136 0.054 Uiso 1 1 calc R . . C45 C 0.6636(6) -0.1524(5) 0.2358(2) 0.0520(13) Uani 1 1 d . . . H45 H 0.6416 -0.2354 0.2309 0.062 Uiso 1 1 calc R . . C46 C 0.7894(6) -0.0755(5) 0.2531(2) 0.0556(14) Uani 1 1 d . . . H46 H 0.8542 -0.1056 0.2599 0.067 Uiso 1 1 calc R . . C47 C 0.8198(5) 0.0441(5) 0.2604(2) 0.0496(13) Uani 1 1 d . . . H47 H 0.9063 0.0957 0.2720 0.060 Uiso 1 1 calc R . . C48 C 0.7279(5) 0.0922(4) 0.25142(18) 0.0405(11) Uani 1 1 d . . . C49 C 0.7643(5) 0.2243(5) 0.2616(2) 0.0506(13) Uani 1 1 d . . . H49A H 0.7405 0.2501 0.2953 0.076 Uiso 1 1 calc R . . H49B H 0.7185 0.2455 0.2350 0.076 Uiso 1 1 calc R . . H49C H 0.8576 0.2631 0.2610 0.076 Uiso 1 1 calc R . . C50 C 0.4780(5) -0.1390(4) 0.09862(16) 0.0374(10) Uani 1 1 d . . . C51 C 0.3472(6) -0.2053(5) 0.0928(2) 0.0531(14) Uani 1 1 d . . . H51 H 0.2870 -0.1691 0.0876 0.064 Uiso 1 1 calc R . . C52 C 0.3034(9) -0.3239(6) 0.0945(3) 0.086(2) Uani 1 1 d . . . H52 H 0.2132 -0.3684 0.0914 0.103 Uiso 1 1 calc R . . C53 C 0.3877(12) -0.3769(6) 0.1007(3) 0.101(3) Uani 1 1 d . . . H53 H 0.3571 -0.4584 0.1021 0.121 Uiso 1 1 calc R . . C54 C 0.5195(10) -0.3123(7) 0.1049(2) 0.084(3) Uani 1 1 d . . . H54 H 0.5784 -0.3506 0.1086 0.101 Uiso 1 1 calc R . . C55 C 0.5669(6) -0.1925(5) 0.10366(18) 0.0540(14) Uani 1 1 d . . . C56 C 0.7095(7) -0.1221(7) 0.1093(2) 0.078(2) Uani 1 1 d . . . H56A H 0.7338 -0.0937 0.0775 0.117 Uiso 1 1 calc R . . H56B H 0.7567 -0.1721 0.1162 0.117 Uiso 1 1 calc R . . H56C H 0.7311 -0.0545 0.1378 0.117 Uiso 1 1 calc R . . C57 C 0.6777(9) 0.3198(8) 0.1482(3) 0.0942(11) Uani 1 1 d . . . C58 C 0.8124(5) 0.3533(5) 0.1587(2) 0.0519(13) Uani 1 1 d . . . C59 C 0.8854(6) 0.4717(6) 0.1787(2) 0.0681(17) Uani 1 1 d . . . H59 H 0.9759 0.4947 0.1867 0.082 Uiso 1 1 calc R . . C60 C 0.8329(7) 0.5555(6) 0.1872(2) 0.073(2) Uani 1 1 d . . . H60 H 0.8855 0.6352 0.2015 0.087 Uiso 1 1 calc R . . C61 C 0.7023(7) 0.5232(5) 0.1749(2) 0.0615(17) Uani 1 1 d . . . H61 H 0.6648 0.5815 0.1800 0.074 Uiso 1 1 calc R . . C62 C 0.6250(5) 0.4064(4) 0.15505(18) 0.0432(11) Uani 1 1 d . . . H62 H 0.5352 0.3855 0.1461 0.052 Uiso 1 1 calc R . . C63 C 0.8778(6) 0.2646(6) 0.1503(2) 0.0674(17) Uani 1 1 d . . . H63A H 0.9021 0.2569 0.1153 0.101 Uiso 1 1 calc R . . H63B H 0.8182 0.1879 0.1554 0.101 Uiso 1 1 calc R . . H63C H 0.9553 0.2917 0.1748 0.101 Uiso 1 1 calc R . . C64 C 0.3628(5) 0.1300(5) 0.02872(17) 0.0942(11) Uani 1 1 d G . . C65 C 0.2392(6) 0.0590(4) 0.03655(17) 0.0942(11) Uani 1 1 d G . . H65 H 0.2173 -0.0235 0.0339 0.113 Uiso 1 1 calc R . . C66 C 0.1476(4) 0.1086(5) 0.04821(17) 0.0942(11) Uani 1 1 d G . . H66 H 0.0632 0.0601 0.0536 0.113 Uiso 1 1 calc R . . C67 C 0.1796(5) 0.2293(5) 0.05204(16) 0.0942(11) Uani 1 1 d G . . H67 H 0.1170 0.2632 0.0600 0.113 Uiso 1 1 calc R . . C68 C 0.3032(5) 0.3003(4) 0.04421(17) 0.0942(11) Uani 1 1 d G . . H68 H 0.3251 0.3828 0.0468 0.113 Uiso 1 1 calc R . . C69 C 0.3948(4) 0.2506(5) 0.03255(17) 0.0942(11) Uani 1 1 d G . . C70 C 0.5184(11) 0.3214(8) 0.0255(3) 0.120(4) Uani 1 1 d . . . H70A H 0.5210 0.4005 0.0236 0.180 Uiso 1 1 calc R . . H70B H 0.5430 0.2870 -0.0065 0.180 Uiso 1 1 calc R . . H70C H 0.5789 0.3266 0.0543 0.180 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02681(15) 0.03867(17) 0.02691(15) 0.00552(12) 0.00267(11) 0.00981(13) Sn2 0.02535(15) 0.03488(17) 0.02798(15) 0.00605(12) 0.00642(11) 0.01013(12) Sn3 0.02706(15) 0.03679(17) 0.02608(15) 0.00639(12) 0.00472(11) 0.01115(12) Sn4 0.03149(16) 0.03508(17) 0.02604(15) 0.00498(12) 0.00262(11) 0.01457(13) Sn5 0.04045(18) 0.03865(19) 0.03675(18) 0.00543(14) 0.01275(14) 0.00968(15) O1 0.0344(16) 0.0350(17) 0.0304(16) 0.0042(13) 0.0107(13) 0.0110(13) O2 0.0272(15) 0.0407(17) 0.0302(15) 0.0090(13) 0.0070(12) 0.0161(13) O3 0.0391(17) 0.0413(18) 0.0295(16) 0.0090(13) 0.0116(13) 0.0213(14) O4 0.0375(17) 0.0282(16) 0.0361(17) 0.0062(13) 0.0146(13) 0.0097(13) O5 0.0297(15) 0.0317(16) 0.0318(16) 0.0060(12) 0.0062(12) 0.0084(13) O6 0.0361(16) 0.0291(16) 0.0327(16) 0.0079(12) 0.0082(13) 0.0128(13) O7 0.0338(16) 0.0479(18) 0.0250(15) 0.0055(13) 0.0041(12) 0.0237(14) O8 0.0438(18) 0.0316(17) 0.0311(16) 0.0049(13) 0.0085(13) 0.0146(14) O9 0.0457(18) 0.0264(16) 0.0320(16) 0.0002(13) 0.0100(14) 0.0034(14) O10 0.056(2) 0.0413(18) 0.0328(17) 0.0027(14) 0.0084(15) 0.0272(16) C1 0.038(2) 0.031(2) 0.042(3) 0.0075(19) 0.019(2) 0.008(2) C2 0.065(4) 0.045(3) 0.039(3) 0.004(2) 0.012(3) 0.002(3) C3 0.055(4) 0.063(4) 0.058(4) 0.008(3) -0.009(3) -0.004(3) C4 0.066(4) 0.048(3) 0.077(4) 0.001(3) 0.015(3) 0.012(3) C5 0.054(3) 0.051(3) 0.050(3) -0.005(3) 0.016(3) 0.004(3) C6 0.046(3) 0.045(3) 0.054(3) 0.016(2) 0.021(2) 0.014(2) C7 0.063(4) 0.055(3) 0.052(3) 0.021(3) 0.019(3) 0.017(3) C8 0.031(2) 0.039(2) 0.033(2) 0.0183(19) 0.0127(18) 0.0153(19) C9 0.048(3) 0.040(3) 0.041(3) 0.016(2) 0.014(2) 0.022(2) C10 0.083(4) 0.059(4) 0.050(3) 0.017(3) 0.026(3) 0.045(3) C11 0.060(4) 0.094(5) 0.069(4) 0.030(4) 0.022(3) 0.054(4) C12 0.038(3) 0.080(4) 0.058(3) 0.028(3) 0.012(2) 0.031(3) C13 0.032(2) 0.051(3) 0.041(3) 0.022(2) 0.011(2) 0.014(2) C14 0.036(3) 0.056(3) 0.054(3) 0.014(3) 0.000(2) 0.007(2) C15 0.035(2) 0.040(3) 0.028(2) 0.0116(18) 0.0160(18) 0.016(2) C16 0.035(2) 0.043(3) 0.036(2) 0.006(2) 0.0099(19) 0.015(2) C17 0.040(3) 0.067(4) 0.043(3) 0.015(3) 0.009(2) 0.028(3) C18 0.059(3) 0.068(4) 0.046(3) 0.014(3) 0.014(3) 0.043(3) C19 0.064(3) 0.045(3) 0.041(3) 0.008(2) 0.020(2) 0.030(3) C20 0.039(3) 0.041(3) 0.030(2) 0.0100(19) 0.0162(19) 0.016(2) C21 0.045(3) 0.043(3) 0.037(3) 0.001(2) 0.008(2) 0.009(2) C22 0.035(2) 0.036(2) 0.026(2) 0.0045(18) 0.0124(18) 0.0101(19) C23 0.044(3) 0.060(3) 0.038(3) 0.006(2) 0.010(2) 0.017(3) C24 0.043(3) 0.073(4) 0.043(3) -0.012(3) 0.005(2) -0.003(3) C25 0.068(4) 0.037(3) 0.075(4) -0.012(3) 0.030(3) 0.002(3) C26 0.069(4) 0.036(3) 0.055(3) 0.007(2) 0.027(3) 0.018(3) C27 0.044(3) 0.035(3) 0.037(2) 0.0098(19) 0.018(2) 0.015(2) C28 0.055(3) 0.059(3) 0.046(3) 0.017(2) 0.016(2) 0.033(3) C29 0.026(2) 0.039(3) 0.032(2) 0.0039(19) 0.0076(18) 0.0056(19) C30 0.037(3) 0.045(3) 0.039(3) 0.011(2) 0.011(2) 0.018(2) C31 0.042(3) 0.070(4) 0.048(3) 0.014(3) 0.001(2) 0.025(3) C32 0.042(3) 0.073(4) 0.047(3) 0.003(3) -0.002(2) 0.015(3) C33 0.046(3) 0.047(3) 0.045(3) -0.005(2) 0.005(2) 0.004(2) C34 0.034(2) 0.037(3) 0.041(3) 0.004(2) 0.011(2) 0.007(2) C35 0.061(4) 0.042(3) 0.060(3) 0.005(3) 0.012(3) 0.022(3) C36 0.046(3) 0.038(3) 0.042(3) 0.020(2) 0.027(2) 0.019(2) C37 0.058(3) 0.056(3) 0.058(3) 0.031(3) 0.024(3) 0.031(3) C38 0.077(4) 0.084(5) 0.090(5) 0.059(4) 0.042(4) 0.055(4) C39 0.112(6) 0.064(5) 0.105(6) 0.049(4) 0.060(5) 0.058(5) C40 0.105(5) 0.037(3) 0.080(5) 0.020(3) 0.053(4) 0.028(3) C41 0.066(4) 0.035(3) 0.053(3) 0.017(2) 0.034(3) 0.016(3) C42 0.072(4) 0.036(3) 0.056(3) 0.002(2) 0.017(3) -0.002(3) C43 0.043(3) 0.049(3) 0.028(2) 0.008(2) 0.0073(19) 0.027(2) C44 0.044(3) 0.050(3) 0.041(3) 0.007(2) 0.007(2) 0.017(2) C45 0.063(4) 0.051(3) 0.052(3) 0.013(3) 0.012(3) 0.031(3) C46 0.059(4) 0.073(4) 0.052(3) 0.018(3) 0.007(3) 0.042(3) C47 0.040(3) 0.064(4) 0.049(3) 0.010(3) 0.003(2) 0.024(3) C48 0.039(3) 0.052(3) 0.033(2) 0.009(2) 0.005(2) 0.020(2) C49 0.046(3) 0.049(3) 0.053(3) 0.008(2) 0.006(2) 0.015(2) C50 0.056(3) 0.034(2) 0.022(2) 0.0036(18) 0.008(2) 0.018(2) C51 0.064(4) 0.041(3) 0.042(3) 0.001(2) 0.012(3) 0.009(3) C52 0.115(6) 0.044(4) 0.061(4) -0.004(3) 0.024(4) -0.009(4) C53 0.202(11) 0.037(4) 0.061(4) 0.011(3) 0.037(6) 0.037(6) C54 0.172(9) 0.067(5) 0.041(3) 0.010(3) 0.010(4) 0.078(6) C55 0.090(4) 0.059(3) 0.028(3) 0.005(2) 0.005(3) 0.047(3) C56 0.087(5) 0.127(6) 0.048(4) 0.009(4) 0.000(3) 0.078(5) C57 0.133(3) 0.133(3) 0.0464(14) -0.0004(16) -0.0007(17) 0.094(3) C58 0.048(3) 0.055(3) 0.045(3) 0.005(2) 0.004(2) 0.012(3) C59 0.057(4) 0.061(4) 0.061(4) -0.003(3) 0.006(3) -0.002(3) C60 0.081(5) 0.046(4) 0.058(4) 0.000(3) 0.018(3) -0.012(3) C61 0.101(5) 0.041(3) 0.044(3) 0.016(2) 0.026(3) 0.023(3) C62 0.052(3) 0.043(3) 0.036(3) 0.013(2) 0.014(2) 0.016(2) C63 0.053(4) 0.086(5) 0.061(4) 0.005(3) 0.002(3) 0.027(3) C64 0.133(3) 0.133(3) 0.0464(14) -0.0004(16) -0.0007(17) 0.094(3) C65 0.133(3) 0.133(3) 0.0464(14) -0.0004(16) -0.0007(17) 0.094(3) C66 0.133(3) 0.133(3) 0.0464(14) -0.0004(16) -0.0007(17) 0.094(3) C67 0.133(3) 0.133(3) 0.0464(14) -0.0004(16) -0.0007(17) 0.094(3) C68 0.133(3) 0.133(3) 0.0464(14) -0.0004(16) -0.0007(17) 0.094(3) C69 0.133(3) 0.133(3) 0.0464(14) -0.0004(16) -0.0007(17) 0.094(3) C70 0.217(12) 0.118(7) 0.034(4) 0.004(4) -0.006(5) 0.081(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O3 2.120(3) . ? Sn1 O1 2.133(3) . ? Sn1 O1 2.365(3) 2_556 ? Sn1 O2 2.389(3) . ? Sn2 O4 2.123(3) . ? Sn2 O2 2.152(3) . ? Sn2 O3 2.349(3) . ? Sn2 O5 2.426(3) . ? Sn3 O5 2.134(3) . ? Sn3 O6 2.149(3) . ? Sn3 O7 2.302(3) . ? Sn3 O4 2.478(3) . ? Sn4 O7 2.142(3) . ? Sn4 O9 2.182(3) . ? Sn4 O8 2.383(3) . ? Sn4 O6 2.423(3) . ? Sn5 O8 2.121(3) . ? Sn5 O10 2.128(3) . ? Sn5 O9 2.359(3) . ? Sn5 O10 2.379(3) 2_655 ? O1 C1 1.385(4) . ? O1 Sn1 2.365(3) 2_556 ? O2 C8 1.378(5) . ? O3 C15 1.372(5) . ? O4 C22 1.373(5) . ? O5 C29 1.381(5) . ? O6 C36 1.374(5) . ? O7 C43 1.387(5) . ? O8 C50 1.368(5) . ? O9 C57 1.377(10) . ? O10 C64 1.361(4) . ? O10 Sn5 2.379(3) 2_655 ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 C7 1.477(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.386(6) . ? C8 C13 1.401(6) . ? C9 C10 1.386(7) . ? C9 H9 0.9500 . ? C10 C11 1.379(9) . ? C10 H10 0.9500 . ? C11 C12 1.362(9) . ? C11 H11 0.9500 . ? C12 C13 1.390(7) . ? C12 H12 0.9500 . ? C13 C14 1.510(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.403(6) . ? C15 C20 1.404(6) . ? C16 C17 1.392(7) . ? C16 H16 0.9500 . ? C17 C18 1.370(8) . ? C17 H17 0.9500 . ? C18 C19 1.377(8) . ? C18 H18 0.9500 . ? C19 C20 1.387(7) . ? C19 H19 0.9500 . ? C20 C21 1.503(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.396(7) . ? C22 C27 1.400(6) . ? C23 C24 1.390(8) . ? C23 H23 0.9500 . ? C24 C25 1.372(9) . ? C24 H24 0.9500 . ? C25 C26 1.364(9) . ? C25 H25 0.9500 . ? C26 C27 1.384(7) . ? C26 H26 0.9500 . ? C27 C28 1.493(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.388(6) . ? C29 C30 1.400(7) . ? C30 C31 1.377(7) . ? C30 H30 0.9500 . ? C31 C32 1.390(8) . ? C31 H31 0.9500 . ? C32 C33 1.372(8) . ? C32 H32 0.9500 . ? C33 C34 1.395(7) . ? C33 H33 0.9500 . ? C34 C35 1.505(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.381(7) . ? C36 C41 1.419(7) . ? C37 C38 1.393(8) . ? C37 H37 0.9500 . ? C38 C39 1.379(11) . ? C38 H38 0.9500 . ? C39 C40 1.358(10) . ? C39 H39 0.9500 . ? C40 C41 1.392(8) . ? C40 H40 0.9500 . ? C41 C42 1.485(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.363(7) . ? C43 C48 1.422(7) . ? C44 C45 1.394(7) . ? C44 H44 0.9500 . ? C45 C46 1.390(8) . ? C45 H45 0.9500 . ? C46 C47 1.372(8) . ? C46 H46 0.9500 . ? C47 C48 1.390(7) . ? C47 H47 0.9500 . ? C48 C49 1.509(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.381(7) . ? C50 C55 1.391(7) . ? C51 C52 1.381(9) . ? C51 H51 0.9500 . ? C52 C53 1.346(12) . ? C52 H52 0.9500 . ? C53 C54 1.389(12) . ? C53 H53 0.9500 . ? C54 C55 1.392(9) . ? C54 H54 0.9500 . ? C55 C56 1.503(9) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C62 1.387(9) . ? C57 C58 1.411(10) . ? C58 C59 1.392(8) . ? C58 C63 1.515(8) . ? C59 C60 1.356(10) . ? C59 H59 0.9500 . ? C60 C61 1.377(9) . ? C60 H60 0.9500 . ? C61 C62 1.388(8) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.3900 . ? C64 C69 1.3900 . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 C67 1.3900 . ? C66 H66 0.9500 . ? C67 C68 1.3900 . ? C67 H67 0.9500 . ? C68 C69 1.3900 . ? C68 H68 0.9500 . ? C69 C70 1.384(11) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sn1 O1 92.59(12) . . ? O3 Sn1 O1 88.91(11) . 2_556 ? O1 Sn1 O1 69.94(12) . 2_556 ? O3 Sn1 O2 69.10(10) . . ? O1 Sn1 O2 88.56(10) . . ? O1 Sn1 O2 148.78(10) 2_556 . ? O4 Sn2 O2 91.54(12) . . ? O4 Sn2 O3 94.38(11) . . ? O2 Sn2 O3 69.39(10) . . ? O4 Sn2 O5 71.41(10) . . ? O2 Sn2 O5 94.17(10) . . ? O3 Sn2 O5 158.38(10) . . ? O5 Sn3 O6 96.05(11) . . ? O5 Sn3 O7 88.84(11) . . ? O6 Sn3 O7 70.25(10) . . ? O5 Sn3 O4 70.18(10) . . ? O6 Sn3 O4 90.21(10) . . ? O7 Sn3 O4 149.93(10) . . ? O7 Sn4 O9 100.67(12) . . ? O7 Sn4 O8 91.56(10) . . ? O9 Sn4 O8 67.50(11) . . ? O7 Sn4 O6 68.00(10) . . ? O9 Sn4 O6 96.92(10) . . ? O8 Sn4 O6 152.18(10) . . ? O8 Sn5 O10 89.18(12) . . ? O8 Sn5 O9 68.91(11) . . ? O10 Sn5 O9 93.56(11) . . ? O8 Sn5 O10 88.50(11) . 2_655 ? O10 Sn5 O10 70.43(13) . 2_655 ? O9 Sn5 O10 152.83(11) . 2_655 ? C1 O1 Sn1 128.2(2) . . ? C1 O1 Sn1 119.0(2) . 2_556 ? Sn1 O1 Sn1 110.05(12) . 2_556 ? C8 O2 Sn2 124.0(2) . . ? C8 O2 Sn1 128.0(2) . . ? Sn2 O2 Sn1 107.77(11) . . ? C15 O3 Sn1 134.7(2) . . ? C15 O3 Sn2 113.8(2) . . ? Sn1 O3 Sn2 110.35(12) . . ? C22 O4 Sn2 131.7(2) . . ? C22 O4 Sn3 119.7(2) . . ? Sn2 O4 Sn3 104.74(11) . . ? C29 O5 Sn3 125.8(2) . . ? C29 O5 Sn2 109.9(2) . . ? Sn3 O5 Sn2 106.17(11) . . ? C36 O6 Sn3 130.6(3) . . ? C36 O6 Sn4 122.8(3) . . ? Sn3 O6 Sn4 105.67(11) . . ? C43 O7 Sn4 134.2(2) . . ? C43 O7 Sn3 114.0(2) . . ? Sn4 O7 Sn3 110.27(12) . . ? C50 O8 Sn5 131.4(3) . . ? C50 O8 Sn4 119.4(3) . . ? Sn5 O8 Sn4 107.14(12) . . ? C57 O9 Sn4 130.3(4) . . ? C57 O9 Sn5 123.5(4) . . ? Sn4 O9 Sn5 105.94(12) . . ? C64 O10 Sn5 131.5(3) . . ? C64 O10 Sn5 117.6(3) . 2_655 ? Sn5 O10 Sn5 109.57(13) . 2_655 ? O1 C1 C2 117.1(2) . . ? O1 C1 C6 122.9(2) . . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 119.9(3) . . ? C1 C6 C7 120.0(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C8 C9 119.6(4) . . ? O2 C8 C13 120.6(4) . . ? C9 C8 C13 119.9(4) . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 120.1(5) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 119.3(5) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 122.5(5) . . ? C11 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C12 C13 C8 117.8(5) . . ? C12 C13 C14 118.8(5) . . ? C8 C13 C14 123.3(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 119.0(4) . . ? O3 C15 C20 121.1(4) . . ? C16 C15 C20 119.8(4) . . ? C17 C16 C15 120.0(5) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 120.4(5) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 119.3(5) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 122.6(5) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C19 C20 C15 117.8(5) . . ? C19 C20 C21 121.6(5) . . ? C15 C20 C21 120.6(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O4 C22 C23 119.3(4) . . ? O4 C22 C27 120.5(4) . . ? C23 C22 C27 120.1(4) . . ? C24 C23 C22 119.6(5) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 120.8(6) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C24 118.7(5) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 123.4(6) . . ? C25 C26 H26 118.3 . . ? C27 C26 H26 118.3 . . ? C26 C27 C22 117.4(5) . . ? C26 C27 C28 121.8(5) . . ? C22 C27 C28 120.8(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 C34 120.6(4) . . ? O5 C29 C30 119.4(4) . . ? C34 C29 C30 120.0(4) . . ? C31 C30 C29 120.6(5) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 119.6(5) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 119.6(5) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 121.8(5) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C29 C34 C33 118.3(5) . . ? C29 C34 C35 121.1(4) . . ? C33 C34 C35 120.6(5) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O6 C36 C37 119.9(5) . . ? O6 C36 C41 119.7(5) . . ? C37 C36 C41 120.3(5) . . ? C36 C37 C38 120.5(6) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C39 C38 C37 119.6(7) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C40 C39 C38 119.8(6) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 123.1(7) . . ? C39 C40 H40 118.5 . . ? C41 C40 H40 118.5 . . ? C40 C41 C36 116.7(6) . . ? C40 C41 C42 121.5(6) . . ? C36 C41 C42 121.6(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 O7 120.0(4) . . ? C44 C43 C48 120.5(4) . . ? O7 C43 C48 119.5(4) . . ? C43 C44 C45 121.0(5) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C46 C45 C44 119.2(5) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C47 C46 C45 119.9(5) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C48 122.1(5) . . ? C46 C47 H47 119.0 . . ? C48 C47 H47 119.0 . . ? C47 C48 C43 117.4(5) . . ? C47 C48 C49 120.4(5) . . ? C43 C48 C49 122.2(4) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O8 C50 C51 119.8(4) . . ? O8 C50 C55 119.9(5) . . ? C51 C50 C55 120.2(5) . . ? C52 C51 C50 120.4(7) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C53 C52 C51 120.4(8) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C54 119.9(7) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C53 C54 C55 121.1(7) . . ? C53 C54 H54 119.4 . . ? C55 C54 H54 119.4 . . ? C50 C55 C54 117.9(7) . . ? C50 C55 C56 121.0(5) . . ? C54 C55 C56 121.1(6) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O9 C57 C62 120.0(7) . . ? O9 C57 C58 120.9(6) . . ? C62 C57 C58 119.0(8) . . ? C59 C58 C57 118.0(6) . . ? C59 C58 C63 119.8(6) . . ? C57 C58 C63 122.2(6) . . ? C60 C59 C58 122.8(6) . . ? C60 C59 H59 118.6 . . ? C58 C59 H59 118.6 . . ? C59 C60 C61 119.0(6) . . ? C59 C60 H60 120.5 . . ? C61 C60 H60 120.5 . . ? C60 C61 C62 120.5(6) . . ? C60 C61 H61 119.7 . . ? C62 C61 H61 119.7 . . ? C57 C62 C61 120.5(6) . . ? C57 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C58 C63 H63A 109.5 . . ? C58 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C58 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O10 C64 C65 117.8(4) . . ? O10 C64 C69 122.1(4) . . ? C65 C64 C69 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 H67 120.0 . . ? C66 C67 H67 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C70 C69 C68 120.1(5) . . ? C70 C69 C64 119.8(5) . . ? C68 C69 C64 120.0 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.676 _refine_diff_density_min -1.369 _refine_diff_density_rms 0.109 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 260 48 ' ' 2 0.137 0.566 0.280 16 1 ' ' 3 0.863 0.434 0.720 16 1 ' ' _platon_squeeze_details ; ; #===END data_9nv052m_0m _database_code_depnum_ccdc_archive 'CCDC 843205' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H88 O8 Sn4' _chemical_formula_weight 1556.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2459(8) _cell_length_b 12.5489(8) _cell_length_c 13.8878(9) _cell_angle_alpha 101.8880(10) _cell_angle_beta 111.3230(10) _cell_angle_gamma 110.8480(10) _cell_volume 1714.48(19) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 8901 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 25.29 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 0.799 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12483 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.30 _reflns_number_total 6145 _reflns_number_gt 5482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.4540P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6145 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.198283(18) 0.115716(16) 0.207095(15) 0.02225(7) Uani 1 1 d . . . Sn2 Sn 0.446334(18) 0.432931(16) 0.349718(15) 0.02161(7) Uani 1 1 d . . . O1 O 0.14802(18) 0.18487(17) 0.08442(15) 0.0269(4) Uani 1 1 d . . . O2 O 0.40084(18) 0.23172(16) 0.25800(15) 0.0230(4) Uani 1 1 d . . . O3 O 0.25826(18) 0.30163(17) 0.32663(15) 0.0230(4) Uani 1 1 d . . . O4 O 0.54771(18) 0.42510(16) 0.50553(15) 0.0229(4) Uani 1 1 d . . . C1 C 0.0264(3) 0.1718(2) 0.0211(2) 0.0253(6) Uani 1 1 d . . . C2 C -0.0852(3) 0.1065(3) 0.0315(2) 0.0300(7) Uani 1 1 d . . . H2 H -0.0776 0.0668 0.0814 0.036 Uiso 1 1 calc R . . C3 C -0.2067(3) 0.0999(3) -0.0311(3) 0.0359(7) Uani 1 1 d . . . H3 H -0.2799 0.0560 -0.0232 0.043 Uiso 1 1 calc R . . C4 C -0.2187(3) 0.1587(3) -0.1055(3) 0.0440(9) Uani 1 1 d . . . H4 H -0.2995 0.1561 -0.1468 0.053 Uiso 1 1 calc R . . C5 C -0.1097(3) 0.2214(3) -0.1176(3) 0.0453(9) Uani 1 1 d . . . H5 H -0.1185 0.2613 -0.1673 0.054 Uiso 1 1 calc R . . C6 C 0.0144(3) 0.2274(3) -0.0579(3) 0.0357(8) Uani 1 1 d . . . C7 C 0.1322(3) 0.2944(4) -0.0731(3) 0.0507(10) Uani 1 1 d . . . H7 H 0.1884 0.2547 -0.0537 0.061 Uiso 1 1 calc R . . C8 C 0.2150(4) 0.4256(4) 0.0053(3) 0.0718(10) Uani 1 1 d . . . H8A H 0.1617 0.4670 -0.0054 0.108 Uiso 1 1 calc R . . H8B H 0.2874 0.4646 -0.0090 0.108 Uiso 1 1 calc R . . H8C H 0.2497 0.4301 0.0809 0.108 Uiso 1 1 calc R . . C9 C 0.0979(4) 0.2833(4) -0.1920(3) 0.0718(10) Uani 1 1 d . . . H9A H 0.0541 0.3316 -0.2113 0.108 Uiso 1 1 calc R . . H9B H 0.0399 0.1983 -0.2420 0.108 Uiso 1 1 calc R . . H9C H 0.1779 0.3129 -0.1982 0.108 Uiso 1 1 calc R . . C10 C 0.4770(3) 0.1868(2) 0.2283(2) 0.0226(6) Uani 1 1 d . . . C11 C 0.5172(3) 0.1135(2) 0.2793(2) 0.0258(6) Uani 1 1 d . . . H11 H 0.4944 0.0974 0.3336 0.031 Uiso 1 1 calc R . . C12 C 0.5905(3) 0.0641(3) 0.2507(3) 0.0306(7) Uani 1 1 d . . . H12 H 0.6173 0.0154 0.2857 0.037 Uiso 1 1 calc R . . C13 C 0.6237(3) 0.0876(3) 0.1695(3) 0.0360(7) Uani 1 1 d . . . H13 H 0.6722 0.0539 0.1489 0.043 Uiso 1 1 calc R . . C14 C 0.5849(3) 0.1611(3) 0.1190(3) 0.0319(7) Uani 1 1 d . . . H14 H 0.6094 0.1774 0.0655 0.038 Uiso 1 1 calc R . . C15 C 0.5102(3) 0.2116(3) 0.1459(2) 0.0256(6) Uani 1 1 d . . . C16 C 0.4716(3) 0.2944(3) 0.0907(3) 0.0334(7) Uani 1 1 d . . . H16 H 0.4006 0.3013 0.1040 0.040 Uiso 1 1 calc R . . C17 C 0.5907(4) 0.4240(4) 0.1449(3) 0.0555(7) Uani 1 1 d . . . H17A H 0.6237 0.4550 0.2244 0.083 Uiso 1 1 calc R . . H17B H 0.5634 0.4780 0.1149 0.083 Uiso 1 1 calc R . . H17C H 0.6597 0.4201 0.1293 0.083 Uiso 1 1 calc R . . C18 C 0.4201(4) 0.2434(4) -0.0351(3) 0.0555(7) Uani 1 1 d . . . H18A H 0.4880 0.2356 -0.0501 0.083 Uiso 1 1 calc R . . H18B H 0.3966 0.2987 -0.0658 0.083 Uiso 1 1 calc R . . H18C H 0.3431 0.1638 -0.0689 0.083 Uiso 1 1 calc R . . C19 C 0.1522(3) 0.3268(3) 0.3098(2) 0.0256(6) Uani 1 1 d . . . C20 C 0.1289(3) 0.3969(3) 0.2467(2) 0.0330(7) Uani 1 1 d . . . H20 H 0.1855 0.4280 0.2180 0.040 Uiso 1 1 calc R . . C21 C 0.0231(3) 0.4208(3) 0.2264(3) 0.0443(9) Uani 1 1 d . . . H21 H 0.0084 0.4682 0.1847 0.053 Uiso 1 1 calc R . . C22 C -0.0609(3) 0.3737(3) 0.2686(3) 0.0514(10) Uani 1 1 d . . . H22 H -0.1326 0.3894 0.2557 0.062 Uiso 1 1 calc R . . C23 C -0.0386(3) 0.3034(3) 0.3298(3) 0.0472(9) Uani 1 1 d . . . H23 H -0.0968 0.2717 0.3570 0.057 Uiso 1 1 calc R . . C24 C 0.0684(3) 0.2777(3) 0.3531(3) 0.0331(7) Uani 1 1 d . . . C25 C 0.0905(3) 0.2000(3) 0.4204(3) 0.0390(8) Uani 1 1 d . . . H25 H 0.1620 0.1843 0.4166 0.047 Uiso 1 1 calc R . . C26 C -0.0322(4) 0.0745(4) 0.3718(4) 0.0801(15) Uani 1 1 d . . . H26A H -0.1029 0.0862 0.3784 0.120 Uiso 1 1 calc R . . H26B H -0.0110 0.0249 0.4122 0.120 Uiso 1 1 calc R . . H26C H -0.0599 0.0335 0.2943 0.120 Uiso 1 1 calc R . . C27 C 0.1375(4) 0.2692(4) 0.5437(3) 0.0635(11) Uani 1 1 d . . . H27A H 0.2159 0.3466 0.5724 0.095 Uiso 1 1 calc R . . H27B H 0.1575 0.2203 0.5854 0.095 Uiso 1 1 calc R . . H27C H 0.0687 0.2842 0.5508 0.095 Uiso 1 1 calc R . . C28 C 0.6155(3) 0.3575(3) 0.5254(2) 0.0255(6) Uani 1 1 d . . . C29 C 0.7231(3) 0.3834(3) 0.5054(3) 0.0337(7) Uani 1 1 d . . . H29 H 0.7456 0.4421 0.4750 0.040 Uiso 1 1 calc R . . C30 C 0.7971(3) 0.3221(3) 0.5304(3) 0.0449(9) Uani 1 1 d . . . H30 H 0.8698 0.3401 0.5175 0.054 Uiso 1 1 calc R . . C31 C 0.7630(4) 0.2343(3) 0.5745(3) 0.0511(10) Uani 1 1 d . . . H31 H 0.8126 0.1929 0.5915 0.061 Uiso 1 1 calc R . . C32 C 0.6553(3) 0.2080(3) 0.5933(3) 0.0416(8) Uani 1 1 d . . . H32 H 0.6337 0.1487 0.6233 0.050 Uiso 1 1 calc R . . C33 C 0.5769(3) 0.2673(3) 0.5688(2) 0.0297(7) Uani 1 1 d . . . C34 C 0.4573(3) 0.2335(3) 0.5879(2) 0.0332(7) Uani 1 1 d . . . H34 H 0.4129 0.2804 0.5601 0.040 Uiso 1 1 calc R . . C35 C 0.3576(4) 0.0962(3) 0.5225(3) 0.0433(8) Uani 1 1 d . . . H35A H 0.3312 0.0759 0.4442 0.065 Uiso 1 1 calc R . . H35B H 0.2808 0.0785 0.5331 0.065 Uiso 1 1 calc R . . H35C H 0.3980 0.0479 0.5489 0.065 Uiso 1 1 calc R . . C36 C 0.4972(4) 0.2686(3) 0.7133(3) 0.0494(9) Uani 1 1 d . . . H36A H 0.5390 0.2222 0.7423 0.074 Uiso 1 1 calc R . . H36B H 0.4193 0.2502 0.7223 0.074 Uiso 1 1 calc R . . H36C H 0.5583 0.3554 0.7533 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02433(11) 0.02136(11) 0.01957(11) 0.00857(8) 0.01018(9) 0.00927(9) Sn2 0.02515(11) 0.02130(11) 0.02093(11) 0.00975(8) 0.01264(9) 0.01094(9) O1 0.0239(10) 0.0309(11) 0.0224(10) 0.0130(9) 0.0076(9) 0.0114(9) O2 0.0236(10) 0.0224(10) 0.0236(10) 0.0067(8) 0.0120(8) 0.0118(8) O3 0.0205(10) 0.0253(10) 0.0233(10) 0.0074(8) 0.0104(8) 0.0120(8) O4 0.0278(10) 0.0215(10) 0.0208(10) 0.0076(8) 0.0103(8) 0.0146(9) C1 0.0256(15) 0.0226(14) 0.0194(14) 0.0044(12) 0.0066(12) 0.0094(12) C2 0.0341(17) 0.0286(16) 0.0211(15) 0.0079(12) 0.0115(13) 0.0114(14) C3 0.0253(16) 0.0348(17) 0.0336(18) 0.0024(14) 0.0118(14) 0.0087(14) C4 0.0289(18) 0.0400(19) 0.050(2) 0.0157(17) 0.0071(16) 0.0163(16) C5 0.0370(19) 0.0390(19) 0.049(2) 0.0243(17) 0.0070(17) 0.0167(16) C6 0.0267(16) 0.0344(17) 0.0293(17) 0.0158(14) 0.0036(14) 0.0060(14) C7 0.0298(18) 0.063(2) 0.045(2) 0.0353(19) 0.0096(16) 0.0078(17) C8 0.066(2) 0.069(2) 0.0444(17) 0.0192(15) 0.0242(15) -0.0011(16) C9 0.066(2) 0.069(2) 0.0444(17) 0.0192(15) 0.0242(15) -0.0011(16) C10 0.0215(14) 0.0193(13) 0.0196(14) 0.0020(11) 0.0077(12) 0.0075(11) C11 0.0245(15) 0.0235(14) 0.0235(15) 0.0068(12) 0.0102(12) 0.0081(12) C12 0.0286(16) 0.0272(15) 0.0342(17) 0.0104(13) 0.0110(14) 0.0162(13) C13 0.0327(17) 0.0370(18) 0.0424(19) 0.0102(15) 0.0210(15) 0.0202(15) C14 0.0348(17) 0.0369(17) 0.0326(17) 0.0140(14) 0.0233(14) 0.0178(14) C15 0.0242(15) 0.0242(14) 0.0249(15) 0.0068(12) 0.0121(13) 0.0091(12) C16 0.0421(19) 0.0388(18) 0.0348(17) 0.0209(15) 0.0249(15) 0.0241(15) C17 0.073(2) 0.0623(18) 0.0601(18) 0.0375(15) 0.0410(16) 0.0442(16) C18 0.073(2) 0.0623(18) 0.0601(18) 0.0375(15) 0.0410(16) 0.0442(16) C19 0.0217(14) 0.0245(15) 0.0215(14) 0.0012(12) 0.0058(12) 0.0107(12) C20 0.0308(17) 0.0312(16) 0.0265(16) 0.0063(13) 0.0081(14) 0.0128(14) C21 0.042(2) 0.040(2) 0.0362(19) 0.0067(16) 0.0025(16) 0.0263(17) C22 0.0313(19) 0.052(2) 0.055(2) 0.0044(19) 0.0077(18) 0.0262(18) C23 0.0301(18) 0.055(2) 0.049(2) 0.0072(18) 0.0205(17) 0.0184(17) C24 0.0262(16) 0.0353(17) 0.0305(17) 0.0045(14) 0.0142(14) 0.0112(14) C25 0.0369(19) 0.045(2) 0.0391(19) 0.0168(16) 0.0249(16) 0.0162(16) C26 0.067(3) 0.066(3) 0.076(3) 0.039(3) 0.024(3) 0.003(2) C27 0.071(3) 0.087(3) 0.043(2) 0.025(2) 0.030(2) 0.045(3) C28 0.0263(15) 0.0240(14) 0.0167(14) 0.0008(11) 0.0027(12) 0.0141(12) C29 0.0299(17) 0.0305(16) 0.0315(17) 0.0001(13) 0.0115(14) 0.0147(14) C30 0.0302(18) 0.042(2) 0.0390(19) -0.0082(16) 0.0048(15) 0.0194(16) C31 0.044(2) 0.047(2) 0.040(2) -0.0031(17) -0.0027(17) 0.0332(19) C32 0.049(2) 0.0351(18) 0.0355(18) 0.0117(15) 0.0079(16) 0.0285(16) C33 0.0353(17) 0.0247(15) 0.0214(15) 0.0050(12) 0.0061(13) 0.0161(13) C34 0.0470(19) 0.0274(16) 0.0294(16) 0.0153(13) 0.0166(15) 0.0210(15) C35 0.054(2) 0.0312(17) 0.041(2) 0.0171(15) 0.0218(17) 0.0163(16) C36 0.075(3) 0.044(2) 0.037(2) 0.0205(17) 0.029(2) 0.030(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.0642(18) . ? Sn1 O2 2.1219(18) . ? Sn1 O3 2.2442(18) . ? Sn2 O4 2.1104(18) . ? Sn2 O3 2.1601(18) . ? Sn2 O2 2.3379(18) . ? Sn2 O4 2.3549(18) 2_666 ? O1 C1 1.354(3) . ? O2 C10 1.384(3) . ? O3 C19 1.394(3) . ? O4 C28 1.384(3) . ? O4 Sn2 2.3550(18) 2_666 ? C1 C2 1.398(4) . ? C1 C6 1.407(4) . ? C2 C3 1.385(4) . ? C2 H2 0.9300 . ? C3 C4 1.384(5) . ? C3 H3 0.9300 . ? C4 C5 1.379(5) . ? C4 H4 0.9300 . ? C5 C6 1.407(4) . ? C5 H5 0.9300 . ? C6 C7 1.505(4) . ? C7 C8 1.481(5) . ? C7 C9 1.510(5) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.388(4) . ? C10 C15 1.403(4) . ? C11 C12 1.378(4) . ? C11 H11 0.9300 . ? C12 C13 1.382(4) . ? C12 H12 0.9300 . ? C13 C14 1.380(4) . ? C13 H13 0.9300 . ? C14 C15 1.393(4) . ? C14 H14 0.9300 . ? C15 C16 1.518(4) . ? C16 C18 1.521(5) . ? C16 C17 1.532(5) . ? C16 H16 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.391(4) . ? C19 C24 1.395(4) . ? C20 C21 1.376(4) . ? C20 H20 0.9300 . ? C21 C22 1.378(5) . ? C21 H21 0.9300 . ? C22 C23 1.373(5) . ? C22 H22 0.9300 . ? C23 C24 1.401(4) . ? C23 H23 0.9300 . ? C24 C25 1.508(4) . ? C25 C26 1.528(5) . ? C25 C27 1.526(5) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.385(4) . ? C28 C33 1.405(4) . ? C29 C30 1.383(4) . ? C29 H29 0.9300 . ? C30 C31 1.379(5) . ? C30 H30 0.9300 . ? C31 C32 1.375(5) . ? C31 H31 0.9300 . ? C32 C33 1.403(4) . ? C32 H32 0.9300 . ? C33 C34 1.510(4) . ? C34 C35 1.529(4) . ? C34 C36 1.542(4) . ? C34 H34 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 O2 87.85(7) . . ? O1 Sn1 O3 85.33(7) . . ? O2 Sn1 O3 72.55(7) . . ? O4 Sn2 O3 90.74(7) . . ? O4 Sn2 O2 89.89(7) . . ? O3 Sn2 O2 70.03(7) . . ? O4 Sn2 O4 69.23(7) . 2_666 ? O3 Sn2 O4 87.22(7) . 2_666 ? O2 Sn2 O4 149.15(6) . 2_666 ? C1 O1 Sn1 126.88(17) . . ? C10 O2 Sn1 121.93(15) . . ? C10 O2 Sn2 131.44(16) . . ? Sn1 O2 Sn2 106.38(7) . . ? C19 O3 Sn2 122.94(16) . . ? C19 O3 Sn1 113.37(15) . . ? Sn2 O3 Sn1 108.42(7) . . ? C28 O4 Sn2 126.12(16) . . ? C28 O4 Sn2 122.75(15) . 2_666 ? Sn2 O4 Sn2 110.77(7) . 2_666 ? O1 C1 C2 122.8(3) . . ? O1 C1 C6 117.4(3) . . ? C2 C1 C6 119.8(3) . . ? C3 C2 C1 121.2(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 122.6(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C1 C6 C5 117.2(3) . . ? C1 C6 C7 120.6(3) . . ? C5 C6 C7 122.1(3) . . ? C8 C7 C6 112.7(3) . . ? C8 C7 C9 110.7(3) . . ? C6 C7 C9 114.4(3) . . ? C8 C7 H7 106.1 . . ? C6 C7 H7 106.1 . . ? C9 C7 H7 106.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 C11 118.9(2) . . ? O2 C10 C15 120.9(2) . . ? C11 C10 C15 120.2(3) . . ? C12 C11 C10 121.1(3) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 119.3(3) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.9(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 121.9(3) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C14 C15 C10 117.5(3) . . ? C14 C15 C16 120.7(3) . . ? C10 C15 C16 121.7(3) . . ? C15 C16 C18 112.8(3) . . ? C15 C16 C17 109.8(3) . . ? C18 C16 C17 109.9(3) . . ? C15 C16 H16 108.0 . . ? C18 C16 H16 108.0 . . ? C17 C16 H16 108.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 O3 119.5(3) . . ? C20 C19 C24 121.1(3) . . ? O3 C19 C24 119.4(3) . . ? C21 C20 C19 120.8(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.3(3) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 122.7(3) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C19 C24 C23 116.3(3) . . ? C19 C24 C25 122.1(3) . . ? C23 C24 C25 121.6(3) . . ? C24 C25 C26 112.2(3) . . ? C24 C25 C27 111.4(3) . . ? C26 C25 C27 111.3(3) . . ? C24 C25 H25 107.2 . . ? C26 C25 H25 107.2 . . ? C27 C25 H25 107.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C28 C29 118.9(3) . . ? O4 C28 C33 119.6(3) . . ? C29 C28 C33 121.4(3) . . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 119.9(3) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 122.4(3) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C32 C33 C28 116.3(3) . . ? C32 C33 C34 120.8(3) . . ? C28 C33 C34 122.9(3) . . ? C33 C34 C35 111.5(3) . . ? C33 C34 C36 112.0(3) . . ? C35 C34 C36 110.2(3) . . ? C33 C34 H34 107.7 . . ? C35 C34 H34 107.7 . . ? C36 C34 H34 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.139 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.077 #===END data_10oc011_0m _database_code_depnum_ccdc_archive 'CCDC 843206' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 O4 Sn2' _chemical_formula_weight 834.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.360(4) _cell_length_b 11.187(5) _cell_length_c 12.069(6) _cell_angle_alpha 63.389(4) _cell_angle_beta 71.234(5) _cell_angle_gamma 84.577(5) _cell_volume 953.9(8) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5854 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 25.22 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6825 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.22 _reflns_number_total 3380 _reflns_number_gt 3223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+0.4537P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3380 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0210 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0480 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.712008(16) 0.558788(13) 0.948934(13) 0.02299(6) Uani 1 1 d . . . O1 O 0.76227(18) 0.37676(14) 1.08271(14) 0.0262(3) Uani 1 1 d . . . O2 O 0.54834(17) 0.45623(13) 0.90673(13) 0.0227(3) Uani 1 1 d . . . C1 C 0.8381(2) 0.3632(2) 1.1711(2) 0.0240(4) Uani 1 1 d . . . C2 C 0.8691(3) 0.4757(2) 1.1861(2) 0.0302(5) Uani 1 1 d . . . H2 H 0.8389 0.5590 1.1335 0.036 Uiso 1 1 calc R . . C3 C 0.9435(3) 0.4660(3) 1.2772(2) 0.0372(6) Uani 1 1 d . . . H3 H 0.9645 0.5422 1.2841 0.045 Uiso 1 1 calc R . . C4 C 0.9858(3) 0.3432(3) 1.3569(2) 0.0384(6) Uani 1 1 d . . . H4 H 1.0344 0.3350 1.4191 0.046 Uiso 1 1 calc R . . C5 C 0.9552(3) 0.2313(2) 1.3436(2) 0.0354(5) Uani 1 1 d . . . H5 H 0.9835 0.1485 1.3988 0.042 Uiso 1 1 calc R . . C6 C 0.8843(3) 0.2367(2) 1.2515(2) 0.0278(5) Uani 1 1 d . . . C7 C 0.8621(3) 0.1109(2) 1.2360(2) 0.0328(5) Uani 1 1 d . . . C8 C 0.9762(3) 0.1304(2) 1.0996(2) 0.0394(6) Uani 1 1 d . . . H8A H 1.0925 0.1394 1.0926 0.059 Uiso 1 1 calc R . . H8B H 0.9476 0.2097 1.0341 0.059 Uiso 1 1 calc R . . H8C H 0.9596 0.0542 1.0870 0.059 Uiso 1 1 calc R . . C9 C 0.6767(3) 0.0836(2) 1.2528(3) 0.0399(6) Uani 1 1 d . . . H9A H 0.6666 0.0029 1.2454 0.060 Uiso 1 1 calc R . . H9B H 0.6417 0.1573 1.1863 0.060 Uiso 1 1 calc R . . H9C H 0.6062 0.0736 1.3372 0.060 Uiso 1 1 calc R . . C10 C 0.9153(4) -0.0144(3) 1.3370(3) 0.0491(7) Uani 1 1 d . . . H10A H 1.0315 -0.0016 1.3283 0.074 Uiso 1 1 calc R . . H10B H 0.9026 -0.0903 1.3227 0.074 Uiso 1 1 calc R . . H10C H 0.8452 -0.0298 1.4232 0.074 Uiso 1 1 calc R . . C11 C 0.5796(2) 0.5001(2) 0.77300(19) 0.0222(4) Uani 1 1 d . . . C12 C 0.5720(3) 0.6362(2) 0.6968(2) 0.0267(5) Uani 1 1 d . . . H12 H 0.5408 0.6929 0.7368 0.032 Uiso 1 1 calc R . . C13 C 0.6097(3) 0.6891(2) 0.5629(2) 0.0325(5) Uani 1 1 d . . . H13 H 0.6028 0.7802 0.5132 0.039 Uiso 1 1 calc R . . C14 C 0.6577(3) 0.6048(2) 0.5043(2) 0.0370(5) Uani 1 1 d . . . H14 H 0.6874 0.6391 0.4141 0.044 Uiso 1 1 calc R . . C15 C 0.6618(3) 0.4688(2) 0.5800(2) 0.0341(5) Uani 1 1 d . . . H15 H 0.6930 0.4134 0.5385 0.041 Uiso 1 1 calc R . . C16 C 0.6211(3) 0.4109(2) 0.7157(2) 0.0251(4) Uani 1 1 d . . . C17 C 0.6180(3) 0.2581(2) 0.7956(2) 0.0295(5) Uani 1 1 d . . . C18 C 0.4401(3) 0.2056(2) 0.8933(3) 0.0434(6) Uani 1 1 d . . . H18A H 0.4339 0.1094 0.9342 0.065 Uiso 1 1 calc R . . H18B H 0.3577 0.2375 0.8481 0.065 Uiso 1 1 calc R . . H18C H 0.4178 0.2370 0.9586 0.065 Uiso 1 1 calc R . . C19 C 0.7485(3) 0.2205(2) 0.8687(3) 0.0412(6) Uani 1 1 d . . . H19A H 0.7416 0.1252 0.9202 0.062 Uiso 1 1 calc R . . H19B H 0.7257 0.2638 0.9247 0.062 Uiso 1 1 calc R . . H19C H 0.8599 0.2490 0.8069 0.062 Uiso 1 1 calc R . . C20 C 0.6573(3) 0.1854(3) 0.7092(3) 0.0424(6) Uani 1 1 d . . . H20A H 0.7695 0.2130 0.6484 0.064 Uiso 1 1 calc R . . H20B H 0.5771 0.2071 0.6622 0.064 Uiso 1 1 calc R . . H20C H 0.6501 0.0904 0.7628 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02110(9) 0.02262(9) 0.02265(9) -0.00788(6) -0.00662(6) 0.00061(6) O1 0.0259(8) 0.0232(7) 0.0310(8) -0.0100(6) -0.0144(6) 0.0042(6) O2 0.0226(7) 0.0246(7) 0.0196(7) -0.0088(6) -0.0065(6) 0.0019(6) C1 0.0146(10) 0.0289(11) 0.0229(11) -0.0076(9) -0.0041(8) -0.0006(8) C2 0.0268(11) 0.0316(12) 0.0332(13) -0.0153(10) -0.0098(10) 0.0042(9) C3 0.0290(12) 0.0509(15) 0.0379(14) -0.0278(12) -0.0051(10) -0.0029(11) C4 0.0266(12) 0.0641(17) 0.0277(12) -0.0229(12) -0.0082(10) 0.0002(11) C5 0.0274(12) 0.0448(14) 0.0237(12) -0.0065(10) -0.0079(9) 0.0019(10) C6 0.0194(10) 0.0315(12) 0.0246(11) -0.0082(9) -0.0028(9) -0.0003(9) C7 0.0278(12) 0.0255(11) 0.0372(13) -0.0069(10) -0.0112(10) 0.0030(9) C8 0.0378(14) 0.0340(13) 0.0470(15) -0.0203(12) -0.0125(11) 0.0088(10) C9 0.0320(13) 0.0291(12) 0.0538(16) -0.0146(11) -0.0123(11) -0.0007(10) C10 0.0470(16) 0.0321(13) 0.0535(17) -0.0041(12) -0.0207(13) 0.0067(11) C11 0.0175(10) 0.0275(11) 0.0201(10) -0.0091(8) -0.0060(8) 0.0005(8) C12 0.0213(10) 0.0275(11) 0.0281(12) -0.0099(9) -0.0074(9) 0.0016(8) C13 0.0298(12) 0.0316(12) 0.0280(12) -0.0045(10) -0.0109(10) -0.0008(9) C14 0.0400(14) 0.0433(14) 0.0213(12) -0.0092(10) -0.0083(10) -0.0015(11) C15 0.0353(13) 0.0411(13) 0.0305(12) -0.0210(11) -0.0082(10) 0.0020(10) C16 0.0201(10) 0.0274(11) 0.0272(11) -0.0115(9) -0.0074(9) 0.0010(8) C17 0.0307(12) 0.0280(11) 0.0307(12) -0.0151(10) -0.0079(10) 0.0024(9) C18 0.0432(15) 0.0258(12) 0.0481(16) -0.0144(11) 0.0010(12) -0.0048(11) C19 0.0500(15) 0.0299(13) 0.0492(15) -0.0171(11) -0.0253(13) 0.0100(11) C20 0.0488(15) 0.0376(14) 0.0462(15) -0.0254(12) -0.0128(12) 0.0070(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.0638(16) . ? Sn1 O2 2.1718(15) . ? Sn1 O2 2.2732(16) 2_667 ? O1 C1 1.355(3) . ? O2 C11 1.399(3) . ? O2 Sn1 2.2732(16) 2_667 ? C1 C2 1.407(3) . ? C1 C6 1.414(3) . ? C2 C3 1.388(3) . ? C2 H2 0.9300 . ? C3 C4 1.372(4) . ? C3 H3 0.9300 . ? C4 C5 1.387(4) . ? C4 H4 0.9300 . ? C5 C6 1.396(3) . ? C5 H5 0.9300 . ? C6 C7 1.535(3) . ? C7 C10 1.533(3) . ? C7 C9 1.539(3) . ? C7 C8 1.541(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.390(3) . ? C11 C16 1.412(3) . ? C12 C13 1.383(3) . ? C12 H12 0.9300 . ? C13 C14 1.376(3) . ? C13 H13 0.9300 . ? C14 C15 1.383(3) . ? C14 H14 0.9300 . ? C15 C16 1.397(3) . ? C15 H15 0.9300 . ? C16 C17 1.538(3) . ? C17 C19 1.531(3) . ? C17 C20 1.532(3) . ? C17 C18 1.537(3) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 O2 89.84(6) . . ? O1 Sn1 O2 89.43(6) . 2_667 ? O2 Sn1 O2 75.04(7) . 2_667 ? C1 O1 Sn1 123.92(13) . . ? C11 O2 Sn1 113.16(11) . . ? C11 O2 Sn1 124.17(11) . 2_667 ? Sn1 O2 Sn1 104.96(6) . 2_667 ? O1 C1 C2 120.02(19) . . ? O1 C1 C6 121.19(19) . . ? C2 C1 C6 118.8(2) . . ? C3 C2 C1 122.0(2) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C4 C3 C2 119.5(2) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 123.3(2) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C5 C6 C1 117.3(2) . . ? C5 C6 C7 121.1(2) . . ? C1 C6 C7 121.6(2) . . ? C10 C7 C6 111.9(2) . . ? C10 C7 C9 107.11(19) . . ? C6 C7 C9 111.59(19) . . ? C10 C7 C8 107.6(2) . . ? C6 C7 C8 108.62(18) . . ? C9 C7 C8 110.0(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 O2 117.64(18) . . ? C12 C11 C16 120.60(19) . . ? O2 C11 C16 121.75(18) . . ? C13 C12 C11 121.5(2) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 118.9(2) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 119.9(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 123.0(2) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C11 116.05(19) . . ? C15 C16 C17 120.77(19) . . ? C11 C16 C17 123.16(19) . . ? C19 C17 C20 107.7(2) . . ? C19 C17 C18 109.9(2) . . ? C20 C17 C18 106.67(19) . . ? C19 C17 C16 110.90(18) . . ? C20 C17 C16 111.99(19) . . ? C18 C17 C16 109.61(18) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.22 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.516 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.059 #===END data_aug183_0m _database_code_depnum_ccdc_archive 'CCDC 843207' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 O4 Sn2, C7 H8' _chemical_formula_sum 'C39 H44 O4 Sn2' _chemical_formula_weight 814.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.8587(11) _cell_length_b 10.8624(8) _cell_length_c 22.5540(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.3940(10) _cell_angle_gamma 90.00 _cell_volume 3624.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9915 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.30 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 1.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25369 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.30 _reflns_number_total 6575 _reflns_number_gt 5689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+2.4893P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6575 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.847961(14) 1.009927(18) 0.047282(10) 0.03335(8) Uani 1 1 d . . . Sn2 Sn 0.738882(15) 0.747858(18) 0.098132(10) 0.03561(8) Uani 1 1 d . . . O1 O 0.94950(14) 0.8829(2) 0.04773(11) 0.0420(5) Uani 1 1 d . . . O2 O 0.61501(15) 0.8265(2) 0.10581(10) 0.0421(5) Uani 1 1 d . . . O3 O 0.80823(14) 0.91410(19) 0.12774(9) 0.0345(5) Uani 1 1 d . . . O4 O 0.75548(13) 0.86223(18) 0.02024(9) 0.0323(5) Uani 1 1 d . . . C1 C 1.0382(2) 0.8726(3) 0.06659(14) 0.0341(7) Uani 1 1 d . . . C2 C 1.0890(2) 0.9690(3) 0.09400(15) 0.0389(7) Uani 1 1 d . . . C3 C 1.1809(2) 0.9502(3) 0.11104(16) 0.0464(8) Uani 1 1 d . . . H3 H 1.2151 1.0143 0.1288 0.056 Uiso 1 1 calc R . . C4 C 1.2220(2) 0.8386(4) 0.10206(16) 0.0497(9) Uani 1 1 d . . . H4 H 1.2834 0.8278 0.1131 0.060 Uiso 1 1 calc R . . C5 C 1.1707(2) 0.7432(3) 0.07639(16) 0.0431(8) Uani 1 1 d . . . H5 H 1.1978 0.6674 0.0709 0.052 Uiso 1 1 calc R . . C6 C 1.0796(2) 0.7581(3) 0.05872(14) 0.0364(7) Uani 1 1 d . . . C7 C 1.0235(2) 0.6524(3) 0.03234(17) 0.0470(8) Uani 1 1 d . . . H7A H 1.0027 0.6709 -0.0083 0.070 Uiso 1 1 calc R . . H7B H 0.9724 0.6400 0.0548 0.070 Uiso 1 1 calc R . . H7C H 1.0596 0.5790 0.0337 0.070 Uiso 1 1 calc R . . C8 C 1.0462(2) 1.0909(3) 0.10739(17) 0.0499(9) Uani 1 1 d . . . H8A H 1.0234 1.1296 0.0708 0.075 Uiso 1 1 calc R . . H8B H 1.0906 1.1432 0.1283 0.075 Uiso 1 1 calc R . . H8C H 0.9974 1.0773 0.1316 0.075 Uiso 1 1 calc R . . C9 C 0.5452(2) 0.7571(3) 0.12203(16) 0.0389(8) Uani 1 1 d . . . C10 C 0.5002(2) 0.6747(3) 0.08144(15) 0.0394(8) Uani 1 1 d . . . C11 C 0.4289(2) 0.6061(3) 0.09940(18) 0.0492(9) Uani 1 1 d . . . H11 H 0.3987 0.5513 0.0728 0.059 Uiso 1 1 calc R . . C12 C 0.4018(2) 0.6175(3) 0.15591(19) 0.0540(10) Uani 1 1 d . . . H12 H 0.3547 0.5696 0.1676 0.065 Uiso 1 1 calc R . . C13 C 0.4454(2) 0.7008(4) 0.19525(17) 0.0510(9) Uani 1 1 d . . . H13 H 0.4263 0.7096 0.2331 0.061 Uiso 1 1 calc R . . C14 C 0.5171(2) 0.7717(3) 0.17921(15) 0.0432(8) Uani 1 1 d . . . C15 C 0.5648(3) 0.8625(4) 0.22151(17) 0.0612(11) Uani 1 1 d . . . H15A H 0.5363 0.8638 0.2580 0.092 Uiso 1 1 calc R . . H15B H 0.5617 0.9430 0.2039 0.092 Uiso 1 1 calc R . . H15C H 0.6270 0.8387 0.2297 0.092 Uiso 1 1 calc R . . C16 C 0.5294(3) 0.6620(3) 0.01973(17) 0.0496(9) Uani 1 1 d . . . H16A H 0.5864 0.6200 0.0216 0.074 Uiso 1 1 calc R . . H16B H 0.5355 0.7422 0.0027 0.074 Uiso 1 1 calc R . . H16C H 0.4849 0.6156 -0.0045 0.074 Uiso 1 1 calc R . . C17 C 0.8323(2) 0.9477(3) 0.18665(14) 0.0365(7) Uani 1 1 d . . . C18 C 0.8973(2) 0.8807(4) 0.22156(15) 0.0471(9) Uani 1 1 d . . . C19 C 0.9183(3) 0.9201(5) 0.28042(17) 0.0681(12) Uani 1 1 d . . . H19 H 0.9602 0.8759 0.3052 0.082 Uiso 1 1 calc R . . C20 C 0.8785(4) 1.0220(5) 0.3021(2) 0.0790(15) Uani 1 1 d . . . H20 H 0.8948 1.0475 0.3410 0.095 Uiso 1 1 calc R . . C21 C 0.8146(3) 1.0871(4) 0.26674(19) 0.0688(13) Uani 1 1 d . . . H21 H 0.7882 1.1563 0.2821 0.083 Uiso 1 1 calc R . . C22 C 0.7888(3) 1.0509(3) 0.20851(16) 0.0473(9) Uani 1 1 d . . . C23 C 0.7176(3) 1.1178(3) 0.17019(19) 0.0623(12) Uani 1 1 d . . . H23A H 0.7445 1.1578 0.1382 0.093 Uiso 1 1 calc R . . H23B H 0.6898 1.1783 0.1936 0.093 Uiso 1 1 calc R . . H23C H 0.6727 1.0603 0.1541 0.093 Uiso 1 1 calc R . . C24 C 0.9449(3) 0.7719(4) 0.19861(19) 0.0622(11) Uani 1 1 d . . . H24A H 0.9049 0.7023 0.1960 0.093 Uiso 1 1 calc R . . H24B H 0.9974 0.7533 0.2252 0.093 Uiso 1 1 calc R . . H24C H 0.9630 0.7903 0.1598 0.093 Uiso 1 1 calc R . . C25 C 0.6996(2) 0.8548(3) -0.03264(13) 0.0331(7) Uani 1 1 d . . . C26 C 0.7130(2) 0.7571(3) -0.07158(15) 0.0392(8) Uani 1 1 d . . . C27 C 0.6558(3) 0.7502(3) -0.12415(17) 0.0548(10) Uani 1 1 d . . . H27 H 0.6625 0.6859 -0.1506 0.066 Uiso 1 1 calc R . . C28 C 0.5898(3) 0.8371(4) -0.13751(17) 0.0604(11) Uani 1 1 d . . . H28 H 0.5530 0.8317 -0.1732 0.072 Uiso 1 1 calc R . . C29 C 0.5774(3) 0.9318(4) -0.09872(17) 0.0519(9) Uani 1 1 d . . . H29 H 0.5318 0.9891 -0.1082 0.062 Uiso 1 1 calc R . . C30 C 0.6324(2) 0.9430(3) -0.04532(14) 0.0377(7) Uani 1 1 d . . . C31 C 0.6176(2) 1.0463(3) -0.00306(16) 0.0440(8) Uani 1 1 d . . . H31A H 0.6654 1.1055 -0.0040 0.066 Uiso 1 1 calc R . . H31B H 0.6172 1.0141 0.0366 0.066 Uiso 1 1 calc R . . H31C H 0.5606 1.0852 -0.0147 0.066 Uiso 1 1 calc R . . C32 C 0.7849(3) 0.6617(3) -0.05645(17) 0.0511(9) Uani 1 1 d . . . H32A H 0.7655 0.6068 -0.0268 0.077 Uiso 1 1 calc R . . H32B H 0.8399 0.7016 -0.0413 0.077 Uiso 1 1 calc R . . H32C H 0.7950 0.6159 -0.0916 0.077 Uiso 1 1 calc R . . C33 C 0.7127(3) 0.4597(3) 0.18079(18) 0.126(3) Uani 1 1 d G . . C34 C 0.8063(3) 0.4526(4) 0.1822(2) 0.104(2) Uani 1 1 d G . . H34 H 0.8422 0.4715 0.2171 0.124 Uiso 1 1 calc R . . C35 C 0.8463(2) 0.4172(4) 0.1316(3) 0.134(3) Uani 1 1 d G . . H35 H 0.9089 0.4125 0.1326 0.161 Uiso 1 1 calc R . . C36 C 0.7927(3) 0.3890(3) 0.0795(2) 0.107(2) Uani 1 1 d G . . H36 H 0.8195 0.3653 0.0457 0.129 Uiso 1 1 calc R . . C37 C 0.6991(3) 0.3961(3) 0.07808(18) 0.113(2) Uani 1 1 d G . . H37 H 0.6633 0.3772 0.0432 0.136 Uiso 1 1 calc R . . C38 C 0.6591(2) 0.4315(3) 0.1287(2) 0.0825(15) Uani 1 1 d G . . H38 H 0.5965 0.4362 0.1277 0.099 Uiso 1 1 calc R . . C39 C 0.6786(8) 0.4964(6) 0.2302(4) 0.199(5) Uani 1 1 d . . . H39A H 0.6871 0.4329 0.2599 0.299 Uiso 1 1 calc R . . H39B H 0.6153 0.5129 0.2218 0.299 Uiso 1 1 calc R . . H39C H 0.7090 0.5700 0.2448 0.299 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.03364(13) 0.02825(12) 0.03882(13) -0.00049(9) 0.00687(9) -0.00131(9) Sn2 0.03896(14) 0.02804(12) 0.03884(14) 0.00379(9) -0.00161(10) -0.00211(9) O1 0.0313(12) 0.0386(12) 0.0562(14) -0.0096(11) 0.0050(10) 0.0021(10) O2 0.0385(13) 0.0369(12) 0.0517(14) 0.0069(10) 0.0090(11) -0.0056(10) O3 0.0389(12) 0.0331(11) 0.0314(11) -0.0006(9) 0.0032(9) -0.0017(9) O4 0.0325(11) 0.0326(11) 0.0313(11) 0.0003(9) 0.0002(9) -0.0024(9) C1 0.0311(16) 0.0373(17) 0.0346(17) 0.0022(13) 0.0071(13) -0.0009(13) C2 0.0382(18) 0.0404(18) 0.0386(18) 0.0044(14) 0.0067(14) -0.0083(14) C3 0.0402(19) 0.050(2) 0.048(2) 0.0056(16) -0.0013(16) -0.0125(16) C4 0.0331(18) 0.057(2) 0.057(2) 0.0151(18) -0.0026(16) -0.0023(16) C5 0.0396(19) 0.0417(19) 0.048(2) 0.0124(15) 0.0061(16) 0.0069(15) C6 0.0375(18) 0.0364(17) 0.0358(17) 0.0060(13) 0.0061(14) -0.0031(13) C7 0.044(2) 0.0373(18) 0.060(2) -0.0012(16) 0.0071(17) 0.0031(15) C8 0.050(2) 0.0409(19) 0.059(2) -0.0133(17) 0.0035(18) -0.0097(16) C9 0.0318(17) 0.0341(17) 0.051(2) 0.0129(14) 0.0041(15) 0.0027(13) C10 0.0362(18) 0.0315(16) 0.050(2) 0.0072(14) 0.0027(15) 0.0022(14) C11 0.0386(19) 0.0402(19) 0.068(3) 0.0062(17) 0.0013(18) -0.0017(15) C12 0.0333(19) 0.049(2) 0.081(3) 0.018(2) 0.0116(19) -0.0055(16) C13 0.044(2) 0.059(2) 0.051(2) 0.0212(19) 0.0140(17) 0.0040(18) C14 0.0415(19) 0.0463(19) 0.0411(19) 0.0132(15) 0.0006(15) 0.0023(15) C15 0.066(3) 0.075(3) 0.042(2) 0.009(2) 0.0020(19) -0.011(2) C16 0.051(2) 0.0403(19) 0.058(2) -0.0066(17) 0.0074(18) -0.0038(16) C17 0.0376(18) 0.0406(18) 0.0325(17) -0.0048(14) 0.0095(14) -0.0139(14) C18 0.043(2) 0.060(2) 0.0381(19) 0.0026(16) 0.0012(15) -0.0099(17) C19 0.064(3) 0.099(4) 0.039(2) 0.002(2) -0.0074(19) -0.027(3) C20 0.094(4) 0.101(4) 0.043(2) -0.023(3) 0.014(3) -0.038(3) C21 0.091(3) 0.065(3) 0.055(3) -0.028(2) 0.035(3) -0.029(3) C22 0.055(2) 0.0409(19) 0.050(2) -0.0090(16) 0.0250(18) -0.0154(17) C23 0.074(3) 0.040(2) 0.079(3) 0.001(2) 0.038(2) 0.011(2) C24 0.057(2) 0.074(3) 0.054(2) 0.012(2) -0.005(2) 0.012(2) C25 0.0339(16) 0.0360(16) 0.0295(16) 0.0032(13) 0.0034(13) -0.0059(13) C26 0.0458(19) 0.0358(17) 0.0358(18) 0.0003(13) 0.0028(15) -0.0034(14) C27 0.073(3) 0.049(2) 0.040(2) -0.0097(16) -0.0065(19) -0.0029(19) C28 0.071(3) 0.060(2) 0.045(2) 0.0002(19) -0.022(2) 0.000(2) C29 0.051(2) 0.052(2) 0.051(2) 0.0118(18) -0.0108(17) 0.0055(18) C30 0.0384(18) 0.0367(17) 0.0381(18) 0.0077(14) 0.0038(14) -0.0008(14) C31 0.0416(19) 0.0392(18) 0.051(2) 0.0045(16) 0.0034(16) 0.0091(15) C32 0.059(2) 0.047(2) 0.048(2) -0.0104(17) 0.0044(18) 0.0111(18) C33 0.247(10) 0.053(3) 0.085(4) 0.022(3) 0.051(6) 0.011(5) C34 0.062(3) 0.091(4) 0.154(6) 0.047(4) -0.009(4) 0.002(3) C35 0.126(6) 0.107(5) 0.159(7) 0.054(5) -0.041(6) -0.010(5) C36 0.116(5) 0.075(4) 0.131(6) 0.026(4) 0.016(5) 0.010(4) C37 0.120(5) 0.069(4) 0.142(6) 0.037(4) -0.034(5) -0.012(4) C38 0.093(4) 0.056(3) 0.095(4) 0.034(3) -0.010(3) -0.005(3) C39 0.362(16) 0.085(5) 0.171(9) 0.035(5) 0.132(10) 0.059(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.044(2) . ? Sn1 O4 2.163(2) . ? Sn1 O3 2.220(2) . ? Sn2 O2 2.051(2) . ? Sn2 O3 2.154(2) . ? Sn2 O4 2.185(2) . ? O1 C1 1.351(4) . ? O2 C9 1.360(4) . ? O3 C17 1.392(4) . ? O4 C25 1.390(3) . ? C1 C2 1.400(4) . ? C1 C6 1.406(4) . ? C2 C3 1.399(5) . ? C2 C8 1.512(5) . ? C3 C4 1.381(5) . ? C3 H3 0.9300 . ? C4 C5 1.382(5) . ? C4 H4 0.9300 . ? C5 C6 1.384(5) . ? C5 H5 0.9300 . ? C6 C7 1.508(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C14 1.401(5) . ? C9 C10 1.404(5) . ? C10 C11 1.387(5) . ? C10 C16 1.502(5) . ? C11 C12 1.378(5) . ? C11 H11 0.9300 . ? C12 C13 1.385(6) . ? C12 H12 0.9300 . ? C13 C14 1.390(5) . ? C13 H13 0.9300 . ? C14 C15 1.503(5) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.393(5) . ? C17 C22 1.406(5) . ? C18 C19 1.402(5) . ? C18 C24 1.494(5) . ? C19 C20 1.367(7) . ? C19 H19 0.9300 . ? C20 C21 1.377(7) . ? C20 H20 0.9300 . ? C21 C22 1.389(5) . ? C21 H21 0.9300 . ? C22 C23 1.491(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.393(4) . ? C25 C26 1.404(4) . ? C26 C27 1.394(5) . ? C26 C32 1.504(5) . ? C27 C28 1.374(5) . ? C27 H27 0.9300 . ? C28 C29 1.374(6) . ? C28 H28 0.9300 . ? C29 C30 1.396(5) . ? C29 H29 0.9300 . ? C30 C31 1.502(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C39 1.329(8) . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 O4 87.12(8) . . ? O1 Sn1 O3 86.12(9) . . ? O4 Sn1 O3 70.85(7) . . ? O2 Sn2 O3 91.81(8) . . ? O2 Sn2 O4 90.06(8) . . ? O3 Sn2 O4 71.68(7) . . ? C1 O1 Sn1 139.06(19) . . ? C9 O2 Sn2 120.32(19) . . ? C17 O3 Sn2 126.04(18) . . ? C17 O3 Sn1 126.39(17) . . ? Sn2 O3 Sn1 107.21(8) . . ? C25 O4 Sn1 126.70(17) . . ? C25 O4 Sn2 123.60(17) . . ? Sn1 O4 Sn2 108.17(8) . . ? O1 C1 C2 123.1(3) . . ? O1 C1 C6 117.3(3) . . ? C2 C1 C6 119.6(3) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C8 119.4(3) . . ? C1 C2 C8 121.6(3) . . ? C4 C3 C2 121.5(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 121.3(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C7 120.9(3) . . ? C1 C6 C7 119.4(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C14 119.0(3) . . ? O2 C9 C10 120.4(3) . . ? C14 C9 C10 120.5(3) . . ? C11 C10 C9 118.8(3) . . ? C11 C10 C16 121.1(3) . . ? C9 C10 C16 120.1(3) . . ? C12 C11 C10 121.3(4) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 119.5(3) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C12 C13 C14 121.3(4) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C9 118.6(3) . . ? C13 C14 C15 121.7(3) . . ? C9 C14 C15 119.7(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C18 120.3(3) . . ? O3 C17 C22 117.3(3) . . ? C18 C17 C22 122.4(3) . . ? C17 C18 C19 117.2(4) . . ? C17 C18 C24 122.9(3) . . ? C19 C18 C24 119.9(4) . . ? C20 C19 C18 121.4(4) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 120.5(4) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 121.0(4) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C17 117.5(4) . . ? C21 C22 C23 121.8(4) . . ? C17 C22 C23 120.6(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 C25 C30 119.7(3) . . ? O4 C25 C26 118.1(3) . . ? C30 C25 C26 122.2(3) . . ? C27 C26 C25 117.5(3) . . ? C27 C26 C32 121.2(3) . . ? C25 C26 C32 121.2(3) . . ? C28 C27 C26 121.0(3) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 120.8(3) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C25 C30 C29 117.8(3) . . ? C25 C30 C31 121.9(3) . . ? C29 C30 C31 120.3(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C39 C33 C34 117.2(6) . . ? C39 C33 C38 122.8(6) . . ? C34 C33 C38 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? C33 C39 H39A 109.5 . . ? C33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.093 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.076 #===END data_aml11jy071ss _database_code_depnum_ccdc_archive 'CCDC 843208' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H75 N O4 Sn2' _chemical_formula_weight 991.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.628(3) _cell_length_b 13.8183(19) _cell_length_c 19.431(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.156(6) _cell_angle_gamma 90.00 _cell_volume 4915.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8236 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44648 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.34 _reflns_number_total 8919 _reflns_number_gt 6267 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.1947P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8919 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.258821(16) 0.66631(2) 0.673872(16) 0.02469(9) Uani 1 1 d . . . Sn2 Sn 0.252948(16) 0.58007(2) 0.844842(15) 0.02390(9) Uani 1 1 d . . . N1 N 0.3721(2) 0.6085(3) 0.6534(2) 0.0377(10) Uani 1 1 d . . . H1 H 0.4016 0.5831 0.6972 0.045 Uiso 1 1 calc R . . O1 O 0.33839(15) 0.7495(2) 0.74740(15) 0.0286(7) Uani 1 1 d . . . O2 O 0.28615(14) 0.54270(18) 0.75183(14) 0.0229(7) Uani 1 1 d . . . O3 O 0.19958(14) 0.67788(18) 0.75936(14) 0.0244(7) Uani 1 1 d . . . O4 O 0.16248(15) 0.49391(19) 0.81811(15) 0.0271(7) Uani 1 1 d . . . C1 C 0.3509(2) 0.8434(3) 0.7694(2) 0.0245(10) Uani 1 1 d . . . C2 C 0.4003(2) 0.8608(3) 0.8418(2) 0.0278(10) Uani 1 1 d . . . C3 C 0.4158(2) 0.9555(3) 0.8662(3) 0.0376(12) Uani 1 1 d . . . H3 H 0.4487 0.9671 0.9137 0.045 Uiso 1 1 calc R . . C4 C 0.3833(3) 1.0327(3) 0.8216(3) 0.0419(13) Uani 1 1 d . . . H4 H 0.3936 1.0959 0.8386 0.050 Uiso 1 1 calc R . . C5 C 0.3355(3) 1.0144(3) 0.7518(3) 0.0389(12) Uani 1 1 d . . . H5 H 0.3130 1.0666 0.7221 0.047 Uiso 1 1 calc R . . C6 C 0.3188(2) 0.9214(3) 0.7228(2) 0.0281(10) Uani 1 1 d . . . C7 C 0.2644(3) 0.9087(3) 0.6447(3) 0.0383(12) Uani 1 1 d . . . H7 H 0.2691 0.8419 0.6301 0.046 Uiso 1 1 calc R . . C8 C 0.2785(3) 0.9747(4) 0.5879(3) 0.0567(16) Uani 1 1 d . . . H8A H 0.2744 1.0411 0.6004 0.085 Uiso 1 1 calc R . . H8B H 0.2433 0.9613 0.5397 0.085 Uiso 1 1 calc R . . H8C H 0.3268 0.9630 0.5880 0.085 Uiso 1 1 calc R . . C9 C 0.1864(3) 0.9207(4) 0.6421(3) 0.0646(18) Uani 1 1 d . . . H9A H 0.1771 0.8744 0.6745 0.097 Uiso 1 1 calc R . . H9B H 0.1530 0.9102 0.5926 0.097 Uiso 1 1 calc R . . H9C H 0.1801 0.9849 0.6576 0.097 Uiso 1 1 calc R . . C10 C 0.4379(2) 0.7768(3) 0.8907(2) 0.0343(11) Uani 1 1 d . . . H10 H 0.4075 0.7193 0.8723 0.041 Uiso 1 1 calc R . . C11 C 0.4458(4) 0.7903(5) 0.9704(3) 0.081(2) Uani 1 1 d . . . H11A H 0.4813 0.8399 0.9924 0.122 Uiso 1 1 calc R . . H11B H 0.4616 0.7307 0.9967 0.122 Uiso 1 1 calc R . . H11C H 0.3996 0.8090 0.9728 0.122 Uiso 1 1 calc R . . C12 C 0.5108(3) 0.7573(4) 0.8845(3) 0.0686(18) Uani 1 1 d . . . H12A H 0.5040 0.7433 0.8340 0.103 Uiso 1 1 calc R . . H12B H 0.5334 0.7030 0.9149 0.103 Uiso 1 1 calc R . . H12C H 0.5414 0.8133 0.9005 0.103 Uiso 1 1 calc R . . C13 C 0.3111(2) 0.4528(3) 0.7395(2) 0.0254(10) Uani 1 1 d . . . C14 C 0.3859(2) 0.4308(3) 0.7733(2) 0.0312(11) Uani 1 1 d . . . C15 C 0.4097(3) 0.3399(3) 0.7597(3) 0.0463(14) Uani 1 1 d . . . H15 H 0.4588 0.3236 0.7815 0.056 Uiso 1 1 calc R . . C16 C 0.3617(3) 0.2743(4) 0.7147(3) 0.0522(15) Uani 1 1 d . . . H16 H 0.3784 0.2139 0.7066 0.063 Uiso 1 1 calc R . . C17 C 0.2888(3) 0.2976(3) 0.6812(3) 0.0436(13) Uani 1 1 d . . . H17 H 0.2571 0.2529 0.6500 0.052 Uiso 1 1 calc R . . C18 C 0.2615(2) 0.3865(3) 0.6930(2) 0.0306(11) Uani 1 1 d . . . C19 C 0.1815(3) 0.4093(3) 0.6547(3) 0.0369(12) Uani 1 1 d . . . H19 H 0.1708 0.4666 0.6788 0.044 Uiso 1 1 calc R . . C20 C 0.1643(3) 0.4352(4) 0.5733(3) 0.0523(15) Uani 1 1 d . . . H20A H 0.1931 0.4899 0.5702 0.079 Uiso 1 1 calc R . . H20B H 0.1134 0.4508 0.5505 0.079 Uiso 1 1 calc R . . H20C H 0.1755 0.3810 0.5484 0.079 Uiso 1 1 calc R . . C21 C 0.1309(3) 0.3289(4) 0.6605(3) 0.0559(15) Uani 1 1 d . . . H21A H 0.1378 0.2727 0.6348 0.084 Uiso 1 1 calc R . . H21B H 0.0811 0.3502 0.6389 0.084 Uiso 1 1 calc R . . H21C H 0.1419 0.3132 0.7115 0.084 Uiso 1 1 calc R . . C22 C 0.4409(2) 0.5028(3) 0.8231(2) 0.0364(12) Uani 1 1 d . . . H22 H 0.4191 0.5674 0.8128 0.044 Uiso 1 1 calc R . . C23 C 0.5120(3) 0.5045(4) 0.8075(3) 0.0554(15) Uani 1 1 d . . . H23A H 0.5373 0.4443 0.8227 0.083 Uiso 1 1 calc R . . H23B H 0.5423 0.5567 0.8344 0.083 Uiso 1 1 calc R . . H23C H 0.5009 0.5137 0.7556 0.083 Uiso 1 1 calc R . . C24 C 0.4584(3) 0.4813(4) 0.9046(3) 0.0605(16) Uani 1 1 d . . . H24A H 0.4146 0.4864 0.9156 0.091 Uiso 1 1 calc R . . H24B H 0.4938 0.5270 0.9340 0.091 Uiso 1 1 calc R . . H24C H 0.4778 0.4170 0.9156 0.091 Uiso 1 1 calc R . . C25 C 0.1378(2) 0.7284(3) 0.7562(2) 0.0228(10) Uani 1 1 d . . . C26 C 0.1432(2) 0.8014(3) 0.8090(2) 0.0259(10) Uani 1 1 d . . . C27 C 0.0791(3) 0.8466(3) 0.8064(3) 0.0338(11) Uani 1 1 d . . . H27 H 0.0811 0.8923 0.8423 0.041 Uiso 1 1 calc R . . C28 C 0.0133(3) 0.8261(3) 0.7528(3) 0.0409(13) Uani 1 1 d . . . H28 H -0.0287 0.8579 0.7524 0.049 Uiso 1 1 calc R . . C29 C 0.0089(2) 0.7581(3) 0.6990(3) 0.0342(11) Uani 1 1 d . . . H29 H -0.0359 0.7459 0.6618 0.041 Uiso 1 1 calc R . . C30 C 0.0706(2) 0.7077(3) 0.7000(2) 0.0275(10) Uani 1 1 d . . . C31 C 0.2155(2) 0.8307(3) 0.8673(2) 0.0317(11) Uani 1 1 d . . . H31 H 0.2546 0.8000 0.8550 0.038 Uiso 1 1 calc R . . C32 C 0.2223(3) 0.7964(4) 0.9446(2) 0.0468(13) Uani 1 1 d . . . H32A H 0.1854 0.8271 0.9586 0.070 Uiso 1 1 calc R . . H32B H 0.2697 0.8132 0.9793 0.070 Uiso 1 1 calc R . . H32C H 0.2161 0.7275 0.9442 0.070 Uiso 1 1 calc R . . C33 C 0.2269(3) 0.9399(3) 0.8682(3) 0.0467(14) Uani 1 1 d . . . H33A H 0.2209 0.9616 0.8194 0.070 Uiso 1 1 calc R . . H33B H 0.2753 0.9553 0.9014 0.070 Uiso 1 1 calc R . . H33C H 0.1917 0.9714 0.8842 0.070 Uiso 1 1 calc R . . C34 C 0.0630(2) 0.6332(3) 0.6406(2) 0.0311(11) Uani 1 1 d . . . H34 H 0.1103 0.6004 0.6535 0.037 Uiso 1 1 calc R . . C35 C 0.0466(3) 0.6799(3) 0.5656(3) 0.0467(13) Uani 1 1 d . . . H35A H 0.0003 0.7125 0.5511 0.070 Uiso 1 1 calc R . . H35B H 0.0447 0.6309 0.5299 0.070 Uiso 1 1 calc R . . H35C H 0.0842 0.7257 0.5684 0.070 Uiso 1 1 calc R . . C36 C 0.0066(3) 0.5562(4) 0.6374(3) 0.0547(15) Uani 1 1 d . . . H36A H 0.0192 0.5260 0.6849 0.082 Uiso 1 1 calc R . . H36B H 0.0057 0.5083 0.6013 0.082 Uiso 1 1 calc R . . H36C H -0.0407 0.5856 0.6240 0.082 Uiso 1 1 calc R . . C37 C 0.1485(2) 0.4484(3) 0.8746(2) 0.0263(10) Uani 1 1 d . . . C38 C 0.0954(2) 0.4873(3) 0.9000(2) 0.0295(10) Uani 1 1 d . . . C39 C 0.0815(3) 0.4385(3) 0.9562(2) 0.0386(12) Uani 1 1 d . . . H39 H 0.0461 0.4629 0.9730 0.046 Uiso 1 1 calc R . . C40 C 0.1181(3) 0.3556(3) 0.9877(3) 0.0420(13) Uani 1 1 d . . . H40 H 0.1081 0.3251 1.0257 0.050 Uiso 1 1 calc R . . C41 C 0.1695(3) 0.3183(3) 0.9623(3) 0.0390(12) Uani 1 1 d . . . H41 H 0.1944 0.2623 0.9839 0.047 Uiso 1 1 calc R . . C42 C 0.1855(2) 0.3617(3) 0.9056(2) 0.0300(11) Uani 1 1 d . . . C43 C 0.2421(3) 0.3165(3) 0.8799(3) 0.0450(13) Uani 1 1 d . . . H43 H 0.2440 0.3546 0.8380 0.054 Uiso 1 1 calc R . . C44 C 0.3181(3) 0.3182(4) 0.9398(4) 0.0745(19) Uani 1 1 d . . . H44A H 0.3305 0.3834 0.9567 0.112 Uiso 1 1 calc R . . H44B H 0.3531 0.2941 0.9200 0.112 Uiso 1 1 calc R . . H44C H 0.3184 0.2782 0.9803 0.112 Uiso 1 1 calc R . . C45 C 0.2213(3) 0.2124(4) 0.8530(3) 0.0704(18) Uani 1 1 d . . . H45A H 0.2203 0.1731 0.8934 0.106 Uiso 1 1 calc R . . H45B H 0.2567 0.1868 0.8343 0.106 Uiso 1 1 calc R . . H45C H 0.1739 0.2121 0.8146 0.106 Uiso 1 1 calc R . . C46 C 0.0537(2) 0.5796(3) 0.8687(2) 0.0338(11) Uani 1 1 d . . . H46 H 0.0751 0.6084 0.8350 0.041 Uiso 1 1 calc R . . C47 C 0.0593(3) 0.6535(3) 0.9289(3) 0.0474(14) Uani 1 1 d . . . H47A H 0.0361 0.6282 0.9609 0.071 Uiso 1 1 calc R . . H47B H 0.0355 0.7124 0.9066 0.071 Uiso 1 1 calc R . . H47C H 0.1098 0.6664 0.9569 0.071 Uiso 1 1 calc R . . C48 C -0.0276(3) 0.5597(4) 0.8247(3) 0.0538(15) Uani 1 1 d . . . H48A H -0.0320 0.5164 0.7847 0.081 Uiso 1 1 calc R . . H48B H -0.0520 0.6195 0.8055 0.081 Uiso 1 1 calc R . . H48C H -0.0496 0.5308 0.8566 0.081 Uiso 1 1 calc R . . C49 C 0.3638(3) 0.5322(4) 0.5982(3) 0.0540(15) Uani 1 1 d . . . H49A H 0.3307 0.5537 0.5510 0.081 Uiso 1 1 calc R . . H49B H 0.3448 0.4748 0.6125 0.081 Uiso 1 1 calc R . . H49C H 0.4105 0.5183 0.5950 0.081 Uiso 1 1 calc R . . C50 C 0.4119(3) 0.6923(4) 0.6399(3) 0.0562(16) Uani 1 1 d . . . H50A H 0.4567 0.6707 0.6355 0.084 Uiso 1 1 calc R . . H50B H 0.4227 0.7368 0.6803 0.084 Uiso 1 1 calc R . . H50C H 0.3824 0.7239 0.5951 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01992(17) 0.02877(17) 0.02283(17) 0.00194(13) 0.00463(13) -0.00188(13) Sn2 0.02068(17) 0.02699(17) 0.02272(17) 0.00134(12) 0.00625(13) 0.00243(13) N1 0.031(2) 0.056(3) 0.026(2) 0.0080(19) 0.0096(19) 0.0028(19) O1 0.0228(17) 0.0281(17) 0.0301(17) -0.0009(13) 0.0035(14) -0.0003(13) O2 0.0224(17) 0.0226(15) 0.0252(16) 0.0017(12) 0.0102(14) 0.0026(12) O3 0.0225(17) 0.0259(16) 0.0276(17) 0.0029(12) 0.0126(14) 0.0053(13) O4 0.0230(17) 0.0340(17) 0.0255(17) 0.0047(13) 0.0103(14) -0.0003(13) C1 0.019(2) 0.028(2) 0.028(2) 0.0006(19) 0.009(2) -0.0024(19) C2 0.020(2) 0.035(3) 0.028(3) -0.0032(19) 0.009(2) -0.0031(19) C3 0.025(3) 0.044(3) 0.038(3) -0.010(2) 0.005(2) -0.006(2) C4 0.041(3) 0.030(3) 0.050(3) -0.010(2) 0.011(3) -0.010(2) C5 0.035(3) 0.026(3) 0.056(4) 0.010(2) 0.017(3) 0.000(2) C6 0.021(2) 0.029(2) 0.033(3) 0.002(2) 0.009(2) -0.003(2) C7 0.033(3) 0.032(3) 0.044(3) 0.010(2) 0.006(2) -0.002(2) C8 0.039(3) 0.075(4) 0.053(4) 0.027(3) 0.012(3) 0.001(3) C9 0.027(3) 0.107(5) 0.052(4) 0.018(3) 0.005(3) -0.015(3) C10 0.029(3) 0.041(3) 0.028(3) -0.002(2) 0.004(2) 0.002(2) C11 0.112(6) 0.099(5) 0.034(3) 0.021(3) 0.028(4) 0.042(4) C12 0.053(4) 0.075(4) 0.082(5) 0.033(3) 0.030(4) 0.026(3) C13 0.027(3) 0.021(2) 0.032(3) 0.0031(18) 0.014(2) 0.0054(19) C14 0.027(3) 0.031(3) 0.037(3) 0.007(2) 0.014(2) 0.006(2) C15 0.037(3) 0.037(3) 0.074(4) 0.013(3) 0.031(3) 0.016(3) C16 0.049(4) 0.029(3) 0.092(5) -0.002(3) 0.041(4) 0.006(3) C17 0.046(3) 0.027(3) 0.069(4) -0.010(2) 0.033(3) -0.007(2) C18 0.033(3) 0.026(2) 0.038(3) -0.007(2) 0.020(2) 0.000(2) C19 0.033(3) 0.036(3) 0.040(3) -0.015(2) 0.012(2) -0.004(2) C20 0.047(4) 0.048(3) 0.050(4) -0.015(3) 0.003(3) 0.003(3) C21 0.036(3) 0.064(4) 0.068(4) -0.014(3) 0.018(3) -0.014(3) C22 0.027(3) 0.047(3) 0.036(3) 0.004(2) 0.011(2) 0.007(2) C23 0.033(3) 0.067(4) 0.067(4) -0.004(3) 0.018(3) 0.005(3) C24 0.055(4) 0.079(4) 0.039(3) 0.015(3) 0.007(3) 0.004(3) C25 0.017(2) 0.022(2) 0.031(3) 0.0097(18) 0.011(2) 0.0057(18) C26 0.024(3) 0.024(2) 0.033(3) 0.0045(19) 0.015(2) 0.0010(19) C27 0.033(3) 0.032(3) 0.039(3) 0.003(2) 0.016(2) 0.008(2) C28 0.027(3) 0.046(3) 0.056(3) 0.012(3) 0.022(3) 0.018(2) C29 0.022(3) 0.042(3) 0.036(3) 0.009(2) 0.007(2) 0.003(2) C30 0.026(3) 0.027(2) 0.030(3) 0.0099(19) 0.010(2) 0.001(2) C31 0.029(3) 0.029(3) 0.037(3) -0.005(2) 0.011(2) -0.003(2) C32 0.048(3) 0.054(3) 0.035(3) -0.003(2) 0.010(3) -0.003(3) C33 0.050(4) 0.035(3) 0.059(4) -0.008(2) 0.023(3) -0.008(2) C34 0.028(3) 0.028(2) 0.034(3) -0.001(2) 0.006(2) -0.003(2) C35 0.049(3) 0.051(3) 0.037(3) 0.004(2) 0.012(3) 0.004(3) C36 0.055(4) 0.048(3) 0.058(4) -0.010(3) 0.016(3) -0.020(3) C37 0.024(3) 0.032(2) 0.020(2) 0.0059(18) 0.003(2) -0.0042(19) C38 0.026(3) 0.032(3) 0.031(3) 0.001(2) 0.011(2) -0.005(2) C39 0.035(3) 0.053(3) 0.033(3) 0.000(2) 0.019(2) -0.009(2) C40 0.042(3) 0.049(3) 0.034(3) 0.013(2) 0.013(3) -0.014(3) C41 0.038(3) 0.036(3) 0.038(3) 0.013(2) 0.006(3) -0.007(2) C42 0.023(3) 0.033(3) 0.032(3) 0.003(2) 0.007(2) -0.004(2) C43 0.043(3) 0.034(3) 0.060(4) 0.012(2) 0.022(3) 0.009(2) C44 0.036(4) 0.093(5) 0.090(5) 0.026(4) 0.018(4) 0.011(3) C45 0.080(5) 0.042(3) 0.100(5) -0.005(3) 0.045(4) 0.010(3) C46 0.031(3) 0.043(3) 0.034(3) 0.007(2) 0.019(2) 0.003(2) C47 0.055(4) 0.044(3) 0.047(3) 0.000(2) 0.023(3) -0.001(3) C48 0.041(3) 0.052(3) 0.059(4) -0.005(3) 0.006(3) 0.011(3) C49 0.072(4) 0.052(3) 0.053(4) 0.004(3) 0.040(3) 0.015(3) C50 0.044(4) 0.077(4) 0.057(4) -0.010(3) 0.031(3) -0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.047(3) . ? Sn1 O2 2.217(3) . ? Sn1 O3 2.352(3) . ? Sn1 N1 2.526(4) . ? Sn2 O4 2.043(3) . ? Sn2 O3 2.104(3) . ? Sn2 O2 2.193(3) . ? N1 C49 1.471(6) . ? N1 C50 1.471(6) . ? N1 H1 0.9100 . ? O1 C1 1.361(5) . ? O2 C13 1.388(4) . ? O3 C25 1.381(4) . ? O4 C37 1.376(5) . ? C1 C6 1.402(6) . ? C1 C2 1.413(6) . ? C2 C3 1.387(6) . ? C2 C10 1.514(6) . ? C3 C4 1.378(6) . ? C3 H3 0.9300 . ? C4 C5 1.365(6) . ? C4 H4 0.9300 . ? C5 C6 1.394(6) . ? C5 H5 0.9300 . ? C6 C7 1.518(6) . ? C7 C9 1.522(7) . ? C7 C8 1.533(6) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.502(7) . ? C10 C11 1.511(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.403(6) . ? C13 C14 1.408(6) . ? C14 C15 1.400(6) . ? C14 C22 1.528(6) . ? C15 C16 1.370(7) . ? C15 H15 0.9300 . ? C16 C17 1.381(7) . ? C16 H16 0.9300 . ? C17 C18 1.391(6) . ? C17 H17 0.9300 . ? C18 C19 1.509(6) . ? C19 C21 1.520(6) . ? C19 C20 1.536(7) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C24 1.525(6) . ? C22 C23 1.531(6) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.406(6) . ? C25 C26 1.415(6) . ? C26 C27 1.389(6) . ? C26 C31 1.517(6) . ? C27 C28 1.365(6) . ? C27 H27 0.9300 . ? C28 C29 1.386(6) . ? C28 H28 0.9300 . ? C29 C30 1.391(6) . ? C29 H29 0.9300 . ? C30 C34 1.514(6) . ? C31 C33 1.524(6) . ? C31 C32 1.533(6) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.518(6) . ? C34 C36 1.520(6) . ? C34 H34 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.411(6) . ? C37 C42 1.417(6) . ? C38 C39 1.390(6) . ? C38 C46 1.519(6) . ? C39 C40 1.374(6) . ? C39 H39 0.9300 . ? C40 C41 1.373(7) . ? C40 H40 0.9300 . ? C41 C42 1.387(6) . ? C41 H41 0.9300 . ? C42 C43 1.509(6) . ? C43 C44 1.524(7) . ? C43 C45 1.535(7) . ? C43 H43 0.9800 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.527(6) . ? C46 C48 1.539(6) . ? C46 H46 0.9800 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 O2 91.16(10) . . ? O1 Sn1 O3 85.18(10) . . ? O2 Sn1 O3 68.23(9) . . ? O1 Sn1 N1 78.13(12) . . ? O2 Sn1 N1 81.64(11) . . ? O3 Sn1 N1 145.16(10) . . ? O4 Sn2 O3 91.96(10) . . ? O4 Sn2 O2 98.21(10) . . ? O3 Sn2 O2 73.26(10) . . ? C49 N1 C50 111.1(4) . . ? C49 N1 Sn1 118.0(3) . . ? C50 N1 Sn1 109.5(3) . . ? C49 N1 H1 105.8 . . ? C50 N1 H1 105.8 . . ? Sn1 N1 H1 105.8 . . ? C1 O1 Sn1 139.5(2) . . ? C13 O2 Sn2 125.6(2) . . ? C13 O2 Sn1 125.8(2) . . ? Sn2 O2 Sn1 108.13(11) . . ? C25 O3 Sn2 122.6(2) . . ? C25 O3 Sn1 130.8(2) . . ? Sn2 O3 Sn1 106.37(11) . . ? C37 O4 Sn2 117.9(2) . . ? O1 C1 C6 122.8(4) . . ? O1 C1 C2 117.1(4) . . ? C6 C1 C2 120.0(4) . . ? C3 C2 C1 119.2(4) . . ? C3 C2 C10 120.8(4) . . ? C1 C2 C10 119.9(4) . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 118.5(4) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 123.4(4) . . ? C4 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C5 C6 C1 117.5(4) . . ? C5 C6 C7 119.3(4) . . ? C1 C6 C7 123.1(4) . . ? C6 C7 C9 110.9(4) . . ? C6 C7 C8 114.0(4) . . ? C9 C7 C8 110.7(4) . . ? C6 C7 H7 107.0 . . ? C9 C7 H7 107.0 . . ? C8 C7 H7 107.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 110.9(5) . . ? C12 C10 C2 110.4(4) . . ? C11 C10 C2 113.2(4) . . ? C12 C10 H10 107.3 . . ? C11 C10 H10 107.3 . . ? C2 C10 H10 107.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 C18 119.3(4) . . ? O2 C13 C14 119.0(4) . . ? C18 C13 C14 121.6(4) . . ? C15 C14 C13 117.9(4) . . ? C15 C14 C22 119.7(4) . . ? C13 C14 C22 122.4(4) . . ? C16 C15 C14 121.1(5) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 120.2(5) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 121.6(5) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C13 117.6(4) . . ? C17 C18 C19 119.8(4) . . ? C13 C18 C19 122.5(4) . . ? C18 C19 C21 113.7(4) . . ? C18 C19 C20 111.1(4) . . ? C21 C19 C20 109.8(4) . . ? C18 C19 H19 107.3 . . ? C21 C19 H19 107.3 . . ? C20 C19 H19 107.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C14 111.9(4) . . ? C24 C22 C23 109.2(4) . . ? C14 C22 C23 111.8(4) . . ? C24 C22 H22 107.9 . . ? C14 C22 H22 107.9 . . ? C23 C22 H22 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 C30 119.6(4) . . ? O3 C25 C26 119.6(4) . . ? C30 C25 C26 120.8(4) . . ? C27 C26 C25 117.7(4) . . ? C27 C26 C31 119.9(4) . . ? C25 C26 C31 122.4(4) . . ? C28 C27 C26 122.0(4) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C28 C29 120.0(4) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 120.8(4) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C25 118.5(4) . . ? C29 C30 C34 119.0(4) . . ? C25 C30 C34 122.5(4) . . ? C26 C31 C33 111.5(4) . . ? C26 C31 C32 112.1(4) . . ? C33 C31 C32 109.5(4) . . ? C26 C31 H31 107.8 . . ? C33 C31 H31 107.8 . . ? C32 C31 H31 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 C35 111.8(4) . . ? C30 C34 C36 112.1(4) . . ? C35 C34 C36 111.0(4) . . ? C30 C34 H34 107.2 . . ? C35 C34 H34 107.2 . . ? C36 C34 H34 107.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O4 C37 C38 119.4(4) . . ? O4 C37 C42 120.4(4) . . ? C38 C37 C42 120.2(4) . . ? C39 C38 C37 118.0(4) . . ? C39 C38 C46 119.5(4) . . ? C37 C38 C46 122.5(4) . . ? C40 C39 C38 122.3(5) . . ? C40 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? C39 C40 C41 119.1(4) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C40 C41 C42 122.0(4) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C41 C42 C37 118.3(4) . . ? C41 C42 C43 119.3(4) . . ? C37 C42 C43 122.4(4) . . ? C42 C43 C44 112.0(5) . . ? C42 C43 C45 111.3(4) . . ? C44 C43 C45 109.9(4) . . ? C42 C43 H43 107.8 . . ? C44 C43 H43 107.8 . . ? C45 C43 H43 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C38 C46 C47 112.0(4) . . ? C38 C46 C48 111.9(4) . . ? C47 C46 C48 108.5(4) . . ? C38 C46 H46 108.1 . . ? C47 C46 H46 108.1 . . ? C48 C46 H46 108.1 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N1 C49 H49A 109.5 . . ? N1 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N1 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N1 C50 H50A 109.5 . . ? N1 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N1 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.775 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.114 #===END data_jun211s _database_code_depnum_ccdc_archive 'CCDC 843209' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H42 O2 Sn' _chemical_formula_sum 'C28 H42 O2 Sn' _chemical_formula_weight 529.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.856(5) _cell_length_b 13.874(5) _cell_length_c 13.921(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.788(5) _cell_angle_gamma 90.00 _cell_volume 2666.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 6146 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 25.39 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.763 _exptl_crystal_size_mid 0.454 _exptl_crystal_size_min 0.349 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_T_max 0.711 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19085 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.42 _reflns_number_total 4919 _reflns_number_gt 4656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+1.5432P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4919 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.603490(9) 0.413490(10) 0.544163(9) 0.03000(6) Uani 1 1 d . . . O1 O 0.71127(9) 0.32595(10) 0.59525(10) 0.0317(3) Uani 1 1 d . . . O2 O 0.52474(9) 0.36977(10) 0.65400(10) 0.0314(3) Uani 1 1 d . . . C1 C 0.79377(13) 0.30767(14) 0.55025(13) 0.0277(4) Uani 1 1 d . . . C2 C 0.87869(14) 0.36191(14) 0.57652(14) 0.0297(4) Uani 1 1 d . . . C3 C 0.95684(15) 0.34903(16) 0.52072(16) 0.0380(5) Uani 1 1 d . . . H3 H 1.0134 0.3855 0.5350 0.046 Uiso 1 1 calc R . . C4 C 0.95365(17) 0.28473(18) 0.44560(17) 0.0443(5) Uani 1 1 d . . . H4 H 1.0057 0.2808 0.4066 0.053 Uiso 1 1 calc R . . C5 C 0.87419(17) 0.22592(17) 0.42739(16) 0.0406(5) Uani 1 1 d . . . H5 H 0.8745 0.1796 0.3781 0.049 Uiso 1 1 calc R . . C6 C 0.79315(14) 0.23331(14) 0.48037(14) 0.0318(4) Uani 1 1 d . . . C7 C 0.70864(16) 0.16156(15) 0.46061(16) 0.0379(5) Uani 1 1 d . . . C8 C 0.6697(2) 0.1250(2) 0.55410(19) 0.0548(6) Uani 1 1 d . . . H8A H 0.6424 0.1784 0.5876 0.082 Uiso 1 1 calc R . . H8B H 0.7222 0.0964 0.5950 0.082 Uiso 1 1 calc R . . H8C H 0.6199 0.0769 0.5387 0.082 Uiso 1 1 calc R . . C9 C 0.62848(18) 0.20685(18) 0.39281(19) 0.0505(6) Uani 1 1 d . . . H9A H 0.5745 0.1623 0.3834 0.076 Uiso 1 1 calc R . . H9B H 0.6534 0.2207 0.3312 0.076 Uiso 1 1 calc R . . H9C H 0.6068 0.2662 0.4209 0.076 Uiso 1 1 calc R . . C10 C 0.7419(2) 0.07142(19) 0.4072(2) 0.0641(8) Uani 1 1 d . . . H10A H 0.6893 0.0252 0.4000 0.096 Uiso 1 1 calc R . . H10B H 0.7970 0.0425 0.4440 0.096 Uiso 1 1 calc R . . H10C H 0.7603 0.0899 0.3441 0.096 Uiso 1 1 calc R . . C11 C 0.88821(15) 0.43153(15) 0.66331(15) 0.0343(5) Uani 1 1 d . . . C12 C 0.8511(2) 0.3845(2) 0.75293(16) 0.0503(6) Uani 1 1 d . . . H12A H 0.7826 0.3707 0.7409 0.075 Uiso 1 1 calc R . . H12B H 0.8612 0.4282 0.8073 0.075 Uiso 1 1 calc R . . H12C H 0.8862 0.3250 0.7673 0.075 Uiso 1 1 calc R . . C13 C 0.83535(17) 0.52714(17) 0.63711(18) 0.0465(6) Uani 1 1 d . . . H13A H 0.7679 0.5140 0.6172 0.070 Uiso 1 1 calc R . . H13B H 0.8655 0.5582 0.5848 0.070 Uiso 1 1 calc R . . H13C H 0.8395 0.5693 0.6929 0.070 Uiso 1 1 calc R . . C14 C 0.99435(17) 0.4597(2) 0.69046(19) 0.0505(6) Uani 1 1 d . . . H14A H 0.9984 0.4983 0.7487 0.076 Uiso 1 1 calc R . . H14B H 1.0185 0.4966 0.6384 0.076 Uiso 1 1 calc R . . H14C H 1.0330 0.4018 0.7014 0.076 Uiso 1 1 calc R . . C15 C 0.43761(14) 0.41406(13) 0.66405(14) 0.0271(4) Uani 1 1 d . . . C16 C 0.35080(14) 0.37160(15) 0.62176(14) 0.0295(4) Uani 1 1 d . . . C17 C 0.26706(15) 0.42807(16) 0.61776(16) 0.0358(5) Uani 1 1 d . . . H17 H 0.2094 0.4032 0.5870 0.043 Uiso 1 1 calc R . . C18 C 0.26623(15) 0.51917(17) 0.65752(16) 0.0389(5) Uani 1 1 d . . . H18 H 0.2106 0.5580 0.6486 0.047 Uiso 1 1 calc R . . C19 C 0.34796(15) 0.55249(15) 0.71057(15) 0.0345(4) Uani 1 1 d . . . H19 H 0.3452 0.6118 0.7428 0.041 Uiso 1 1 calc R . . C20 C 0.43479(14) 0.50054(14) 0.71780(14) 0.0284(4) Uani 1 1 d . . . C21 C 0.34585(16) 0.26633(15) 0.58611(15) 0.0359(5) Uani 1 1 d . . . C22 C 0.3897(2) 0.19989(18) 0.6660(2) 0.0659(8) Uani 1 1 d . . . H22A H 0.3873 0.1337 0.6434 0.099 Uiso 1 1 calc R . . H22B H 0.3531 0.2057 0.7222 0.099 Uiso 1 1 calc R . . H22C H 0.4565 0.2182 0.6831 0.099 Uiso 1 1 calc R . . C23 C 0.3989(3) 0.2515(2) 0.4956(2) 0.0783(10) Uani 1 1 d . . . H23A H 0.3720 0.2942 0.4451 0.117 Uiso 1 1 calc R . . H23B H 0.3913 0.1851 0.4744 0.117 Uiso 1 1 calc R . . H23C H 0.4671 0.2656 0.5098 0.117 Uiso 1 1 calc R . . C24 C 0.2410(2) 0.2335(2) 0.5619(3) 0.0758(10) Uani 1 1 d . . . H24A H 0.2123 0.2704 0.5077 0.114 Uiso 1 1 calc R . . H24B H 0.2043 0.2436 0.6174 0.114 Uiso 1 1 calc R . . H24C H 0.2402 0.1655 0.5454 0.114 Uiso 1 1 calc R . . C25 C 0.52174(15) 0.53682(15) 0.78491(15) 0.0336(4) Uani 1 1 d . . . C26 C 0.5611(2) 0.4567(2) 0.8516(2) 0.0675(8) Uani 1 1 d . . . H26A H 0.5810 0.4028 0.8135 0.101 Uiso 1 1 calc R . . H26B H 0.5110 0.4358 0.8916 0.101 Uiso 1 1 calc R . . H26C H 0.6163 0.4804 0.8922 0.101 Uiso 1 1 calc R . . C27 C 0.6012(2) 0.5765(3) 0.7285(2) 0.0761(11) Uani 1 1 d . . . H27A H 0.6459 0.6138 0.7710 0.114 Uiso 1 1 calc R . . H27B H 0.5732 0.6176 0.6771 0.114 Uiso 1 1 calc R . . H27C H 0.6356 0.5237 0.7010 0.114 Uiso 1 1 calc R . . C28 C 0.4921(2) 0.6191(3) 0.8499(2) 0.0723(9) Uani 1 1 d . . . H28A H 0.5462 0.6358 0.8955 0.108 Uiso 1 1 calc R . . H28B H 0.4377 0.5987 0.8846 0.108 Uiso 1 1 calc R . . H28C H 0.4735 0.6749 0.8106 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02596(9) 0.03269(9) 0.03148(9) -0.00001(5) 0.00318(6) 0.00335(5) O1 0.0250(7) 0.0362(8) 0.0341(7) -0.0005(6) 0.0031(5) 0.0057(6) O2 0.0267(7) 0.0324(7) 0.0355(8) -0.0001(6) 0.0056(6) 0.0026(6) C1 0.0266(9) 0.0315(10) 0.0250(9) 0.0043(8) 0.0017(7) 0.0067(8) C2 0.0293(10) 0.0314(10) 0.0278(10) 0.0051(8) -0.0011(8) 0.0045(8) C3 0.0304(10) 0.0433(12) 0.0406(12) 0.0070(10) 0.0048(9) 0.0003(9) C4 0.0408(12) 0.0522(14) 0.0424(13) 0.0039(10) 0.0175(10) 0.0072(10) C5 0.0501(13) 0.0420(12) 0.0304(11) -0.0025(9) 0.0072(9) 0.0108(10) C6 0.0341(10) 0.0313(10) 0.0291(10) 0.0023(8) -0.0025(8) 0.0073(8) C7 0.0429(12) 0.0313(11) 0.0380(12) -0.0033(9) -0.0059(9) 0.0019(9) C8 0.0602(16) 0.0486(15) 0.0543(15) 0.0075(12) -0.0027(12) -0.0188(13) C9 0.0519(14) 0.0445(13) 0.0518(14) -0.0054(11) -0.0158(11) 0.0025(11) C10 0.0686(19) 0.0391(14) 0.083(2) -0.0197(14) -0.0018(16) 0.0019(13) C11 0.0336(11) 0.0358(11) 0.0323(11) 0.0000(9) -0.0035(9) -0.0015(9) C12 0.0627(16) 0.0585(15) 0.0293(12) -0.0034(11) 0.0007(11) -0.0103(13) C13 0.0446(13) 0.0417(13) 0.0518(14) -0.0084(11) -0.0044(11) -0.0002(10) C14 0.0419(13) 0.0551(15) 0.0517(15) -0.0010(12) -0.0126(11) -0.0047(11) C15 0.0261(10) 0.0297(10) 0.0258(10) 0.0040(7) 0.0039(8) -0.0003(7) C16 0.0298(10) 0.0323(10) 0.0266(10) 0.0024(8) 0.0029(8) -0.0058(8) C17 0.0257(10) 0.0452(12) 0.0359(11) 0.0035(9) -0.0013(8) -0.0069(9) C18 0.0296(10) 0.0448(13) 0.0427(12) 0.0027(10) 0.0054(9) 0.0079(9) C19 0.0369(11) 0.0328(11) 0.0348(11) -0.0022(9) 0.0080(9) 0.0026(9) C20 0.0280(9) 0.0312(10) 0.0266(10) 0.0013(8) 0.0062(8) -0.0029(8) C21 0.0416(12) 0.0321(11) 0.0338(11) -0.0013(9) 0.0011(9) -0.0094(9) C22 0.098(2) 0.0327(13) 0.0627(18) 0.0040(12) -0.0175(16) -0.0104(14) C23 0.122(3) 0.0551(17) 0.0639(18) -0.0265(15) 0.0415(18) -0.0359(18) C24 0.0567(17) 0.0476(16) 0.120(3) -0.0149(17) -0.0131(17) -0.0204(13) C25 0.0331(10) 0.0369(11) 0.0307(10) -0.0043(9) 0.0018(8) -0.0065(9) C26 0.077(2) 0.0593(17) 0.0594(17) 0.0061(14) -0.0328(15) -0.0151(15) C27 0.067(2) 0.117(3) 0.0439(15) -0.0077(16) 0.0070(14) -0.0588(19) C28 0.0579(17) 0.086(2) 0.071(2) -0.0454(18) -0.0107(15) 0.0005(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.0084(14) . ? Sn1 O2 2.0433(14) . ? O1 C1 1.372(2) . ? O2 C15 1.372(2) . ? C1 C6 1.418(3) . ? C1 C2 1.419(3) . ? C2 C3 1.396(3) . ? C2 C11 1.544(3) . ? C3 C4 1.373(3) . ? C3 H3 0.9400 . ? C4 C5 1.377(3) . ? C4 H4 0.9400 . ? C5 C6 1.398(3) . ? C5 H5 0.9400 . ? C6 C7 1.544(3) . ? C7 C9 1.531(3) . ? C7 C8 1.536(3) . ? C7 C10 1.545(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 C12 1.534(3) . ? C11 C14 1.538(3) . ? C11 C13 1.544(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C20 1.416(3) . ? C15 C16 1.422(3) . ? C16 C17 1.397(3) . ? C16 C21 1.542(3) . ? C17 C18 1.380(3) . ? C17 H17 0.9400 . ? C18 C19 1.379(3) . ? C18 H18 0.9400 . ? C19 C20 1.399(3) . ? C19 H19 0.9400 . ? C20 C25 1.546(3) . ? C21 C23 1.524(3) . ? C21 C22 1.531(3) . ? C21 C24 1.533(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C27 1.509(3) . ? C25 C26 1.520(3) . ? C25 C28 1.534(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 O2 89.04(6) . . ? C1 O1 Sn1 124.98(12) . . ? C15 O2 Sn1 118.21(11) . . ? O1 C1 C6 119.36(17) . . ? O1 C1 C2 119.27(17) . . ? C6 C1 C2 121.35(17) . . ? C3 C2 C1 117.00(19) . . ? C3 C2 C11 119.73(18) . . ? C1 C2 C11 123.26(17) . . ? C4 C3 C2 122.0(2) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 120.0(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 121.6(2) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 117.16(19) . . ? C5 C6 C7 119.30(19) . . ? C1 C6 C7 123.54(18) . . ? C9 C7 C8 111.7(2) . . ? C9 C7 C6 110.21(18) . . ? C8 C7 C6 112.15(18) . . ? C9 C7 C10 105.4(2) . . ? C8 C7 C10 106.3(2) . . ? C6 C7 C10 110.8(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C14 106.64(19) . . ? C12 C11 C2 110.98(18) . . ? C14 C11 C2 111.63(18) . . ? C12 C11 C13 111.9(2) . . ? C14 C11 C13 105.37(18) . . ? C2 C11 C13 110.17(17) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C20 119.77(17) . . ? O2 C15 C16 119.56(17) . . ? C20 C15 C16 120.66(18) . . ? C17 C16 C15 117.08(18) . . ? C17 C16 C21 120.25(18) . . ? C15 C16 C21 122.60(18) . . ? C18 C17 C16 122.15(19) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C19 C18 C17 119.2(2) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 121.9(2) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C20 C15 117.38(18) . . ? C19 C20 C25 119.87(18) . . ? C15 C20 C25 122.73(17) . . ? C23 C21 C22 109.2(2) . . ? C23 C21 C24 107.0(2) . . ? C22 C21 C24 107.0(2) . . ? C23 C21 C16 112.50(18) . . ? C22 C21 C16 109.39(18) . . ? C24 C21 C16 111.6(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 110.2(2) . . ? C27 C25 C28 106.2(2) . . ? C26 C25 C28 106.5(2) . . ? C27 C25 C20 111.71(18) . . ? C26 C25 C20 110.64(18) . . ? C28 C25 C20 111.40(18) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.42 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.380 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.052 #===END data_9ap291ne _database_code_depnum_ccdc_archive 'CCDC 843210' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 O8 Sn6, 2(C5 H5 N)' _chemical_formula_sum 'C46 H54 N2 O8 Sn6' _chemical_formula_weight 1475.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.9836(18) _cell_length_b 19.1076(18) _cell_length_c 15.9975(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.263(2) _cell_angle_gamma 90.00 _cell_volume 4877.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9887 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.25 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 3.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5781 _exptl_absorpt_correction_T_max 0.6388 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15830 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.24 _reflns_number_total 4370 _reflns_number_gt 3933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4370 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.363737(17) 0.663374(13) 0.322902(19) 0.02762(13) Uani 1 1 d . . . Sn2 Sn 0.5000 0.796481(17) 0.2500 0.02356(14) Uani 1 2 d S . . Sn3 Sn 0.581664(17) 0.667751(11) 0.387814(17) 0.02358(13) Uani 1 1 d . . . Sn4 Sn 0.5000 0.535312(17) 0.2500 0.02574(14) Uani 1 2 d S . . N1 N 0.2096(2) 0.73852(19) 0.2346(3) 0.0505(10) Uani 1 1 d . . . O1 O 0.36087(14) 0.58067(12) 0.20910(15) 0.0266(5) Uani 1 1 d . . . O2 O 0.47465(14) 0.75213(12) 0.38732(15) 0.0247(5) Uani 1 1 d . . . O3 O 0.40895(14) 0.72042(12) 0.22495(14) 0.0222(5) Uani 1 1 d . . . O4 O 0.47839(13) 0.61020(12) 0.33934(14) 0.0231(5) Uani 1 1 d . . . C1 C 0.2927(2) 0.53981(17) 0.1846(2) 0.0234(7) Uani 1 1 d . . . C2 C 0.2191(2) 0.5459(2) 0.2273(3) 0.0330(9) Uani 1 1 d . . . H2 H 0.2175 0.5770 0.2719 0.040 Uiso 1 1 calc R . . C3 C 0.1494(2) 0.5071(2) 0.2049(3) 0.0341(9) Uani 1 1 d . . . H3 H 0.1013 0.5118 0.2345 0.041 Uiso 1 1 calc R . . C4 C 0.1506(2) 0.4604(2) 0.1379(3) 0.0406(10) Uani 1 1 d . . . H4 H 0.1036 0.4335 0.1230 0.049 Uiso 1 1 calc R . . C5 C 0.2213(2) 0.4548(2) 0.0945(3) 0.0369(9) Uani 1 1 d . . . H5 H 0.2213 0.4242 0.0493 0.044 Uiso 1 1 calc R . . C6 C 0.2944(2) 0.49361(18) 0.1156(2) 0.0290(8) Uani 1 1 d . . . C7 C 0.3701(3) 0.4831(2) 0.0638(3) 0.0345(9) Uani 1 1 d . . . H7 H 0.4153 0.5131 0.0874 0.041 Uiso 1 1 calc R . . C8 C 0.3516(3) 0.5050(2) -0.0276(3) 0.0438(11) Uani 1 1 d . . . H8A H 0.3997 0.4956 -0.0591 0.066 Uiso 1 1 calc . . . H8B H 0.3392 0.5541 -0.0300 0.066 Uiso 1 1 calc . . . H8C H 0.3045 0.4790 -0.0509 0.066 Uiso 1 1 calc . . . C9 C 0.4009(3) 0.4075(2) 0.0685(3) 0.0476(11) Uani 1 1 d . . . H9A H 0.4129 0.3947 0.1259 0.071 Uiso 1 1 calc . . . H9B H 0.4507 0.4030 0.0382 0.071 Uiso 1 1 calc . . . H9C H 0.3582 0.3771 0.0442 0.071 Uiso 1 1 calc . . . C10 C 0.4629(2) 0.79297(18) 0.4560(2) 0.0246(7) Uani 1 1 d . . . C11 C 0.3906(2) 0.7844(2) 0.4981(2) 0.0314(8) Uani 1 1 d . . . H11 H 0.3510 0.7517 0.4788 0.038 Uiso 1 1 calc R . . C12 C 0.3758(3) 0.8237(2) 0.5683(3) 0.0367(10) Uani 1 1 d . . . H12 H 0.3272 0.8164 0.5964 0.044 Uiso 1 1 calc R . . C13 C 0.4330(3) 0.8737(2) 0.5969(3) 0.0399(10) Uani 1 1 d . . . H13 H 0.4233 0.9006 0.6439 0.048 Uiso 1 1 calc R . . C14 C 0.5053(3) 0.8828(2) 0.5538(3) 0.0383(9) Uani 1 1 d . . . H14 H 0.5436 0.9169 0.5724 0.046 Uiso 1 1 calc R . . C15 C 0.5230(3) 0.84312(18) 0.4835(2) 0.0276(8) Uani 1 1 d . . . C16 C 0.6039(2) 0.8561(2) 0.4430(2) 0.0328(9) Uani 1 1 d . . . H16 H 0.6049 0.8247 0.3946 0.039 Uiso 1 1 calc R . . C17 C 0.6100(3) 0.9309(2) 0.4099(3) 0.0445(11) Uani 1 1 d . . . H17A H 0.5638 0.9399 0.3703 0.067 Uiso 1 1 calc . . . H17B H 0.6617 0.9366 0.3830 0.067 Uiso 1 1 calc . . . H17C H 0.6082 0.9633 0.4557 0.067 Uiso 1 1 calc . . . C18 C 0.6812(3) 0.8387(2) 0.5007(3) 0.0416(11) Uani 1 1 d . . . H18A H 0.6839 0.8701 0.5477 0.062 Uiso 1 1 calc . . . H18B H 0.7309 0.8438 0.4702 0.062 Uiso 1 1 calc . . . H18C H 0.6773 0.7914 0.5203 0.062 Uiso 1 1 calc . . . C19 C 0.2316(3) 0.8064(3) 0.2401(4) 0.0528(13) Uani 1 1 d . . . H19 H 0.2840 0.8172 0.2649 0.063 Uiso 1 1 calc R . . C20 C 0.1818(3) 0.8604(3) 0.2115(3) 0.0489(11) Uani 1 1 d . . . H20 H 0.2001 0.9065 0.2161 0.059 Uiso 1 1 calc R . . C21 C 0.1037(3) 0.8445(3) 0.1756(4) 0.0534(14) Uani 1 1 d . . . H21 H 0.0683 0.8798 0.1549 0.064 Uiso 1 1 calc R . . C22 C 0.0789(3) 0.7764(3) 0.1710(3) 0.0487(11) Uani 1 1 d . . . H22 H 0.0261 0.7645 0.1479 0.058 Uiso 1 1 calc R . . C23 C 0.1340(3) 0.7252(2) 0.2012(3) 0.0459(10) Uani 1 1 d . . . H23 H 0.1166 0.6788 0.1978 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02166(19) 0.0332(2) 0.0286(2) 0.00734(10) 0.00669(14) 0.00453(9) Sn2 0.0232(2) 0.0194(2) 0.0276(2) 0.000 -0.00299(16) 0.000 Sn3 0.02365(19) 0.02552(19) 0.0210(2) 0.00172(8) -0.00357(13) -0.00147(8) Sn4 0.0320(2) 0.0192(2) 0.0258(2) 0.000 -0.00047(17) 0.000 N1 0.048(2) 0.042(2) 0.060(3) 0.0074(18) -0.0128(19) 0.0027(17) O1 0.0227(12) 0.0250(12) 0.0318(14) -0.0020(10) -0.0005(10) -0.0046(10) O2 0.0242(12) 0.0255(12) 0.0246(13) -0.0050(10) 0.0018(10) -0.0002(9) O3 0.0204(11) 0.0249(12) 0.0212(12) 0.0011(9) 0.0006(9) 0.0006(10) O4 0.0213(12) 0.0238(12) 0.0241(12) -0.0003(10) 0.0004(10) -0.0001(9) C1 0.0230(17) 0.0220(17) 0.0253(18) 0.0013(14) 0.0016(14) -0.0015(13) C2 0.0303(19) 0.034(2) 0.035(2) -0.0041(16) 0.0003(16) 0.0018(16) C3 0.0219(18) 0.041(2) 0.039(2) 0.0072(18) 0.0038(16) -0.0015(16) C4 0.029(2) 0.041(2) 0.051(3) -0.0027(19) -0.0052(19) -0.0113(17) C5 0.034(2) 0.032(2) 0.043(2) -0.0096(17) -0.0048(18) -0.0055(16) C6 0.0279(19) 0.0298(18) 0.029(2) 0.0008(15) -0.0022(15) -0.0007(15) C7 0.034(2) 0.035(2) 0.034(2) -0.0124(17) -0.0041(17) 0.0016(17) C8 0.052(3) 0.045(2) 0.034(2) -0.0080(18) 0.000(2) 0.006(2) C9 0.049(3) 0.044(3) 0.049(3) -0.010(2) -0.004(2) 0.013(2) C10 0.0293(18) 0.0210(16) 0.0232(18) -0.0001(13) 0.0007(15) 0.0066(14) C11 0.0294(19) 0.0322(19) 0.032(2) -0.0010(16) 0.0007(16) 0.0000(15) C12 0.035(2) 0.047(2) 0.030(2) 0.0012(18) 0.0136(19) 0.0064(18) C13 0.044(2) 0.046(2) 0.031(2) -0.0145(18) 0.0112(18) 0.0061(19) C14 0.046(2) 0.032(2) 0.035(2) -0.0102(17) -0.0052(19) 0.0025(17) C15 0.033(2) 0.0270(18) 0.0227(19) -0.0018(14) 0.0001(16) 0.0046(15) C16 0.033(2) 0.0323(19) 0.032(2) -0.0065(17) -0.0064(17) -0.0025(17) C17 0.046(3) 0.042(2) 0.046(3) 0.006(2) 0.003(2) -0.004(2) C18 0.033(2) 0.046(3) 0.044(3) -0.0011(18) -0.008(2) -0.0038(17) C19 0.036(2) 0.049(3) 0.072(4) -0.007(2) -0.009(2) 0.004(2) C20 0.045(3) 0.037(2) 0.065(3) -0.010(2) 0.006(2) 0.002(2) C21 0.052(3) 0.044(3) 0.062(3) -0.007(2) -0.010(3) 0.020(2) C22 0.041(2) 0.057(3) 0.047(3) -0.007(2) -0.006(2) -0.001(2) C23 0.051(3) 0.040(2) 0.046(3) 0.0032(19) -0.004(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O3 2.072(2) . ? Sn1 O4 2.099(2) . ? Sn1 O1 2.409(2) . ? Sn2 O3 2.079(2) 2_655 ? Sn2 O3 2.079(2) . ? Sn2 O2 2.410(2) 2_655 ? Sn2 O2 2.410(2) . ? Sn3 O3 2.079(2) 2_655 ? Sn3 O4 2.095(2) . ? Sn3 O2 2.350(2) . ? Sn3 O1 2.486(2) 2_655 ? Sn4 O4 2.065(2) . ? Sn4 O4 2.065(2) 2_655 ? Sn4 O1 2.441(2) 2_655 ? Sn4 O1 2.441(2) . ? N1 C23 1.317(5) . ? N1 C19 1.345(6) . ? O1 C1 1.380(4) . ? O1 Sn3 2.486(2) 2_655 ? O2 C10 1.370(4) . ? O3 Sn3 2.079(2) 2_655 ? C1 C2 1.398(5) . ? C1 C6 1.414(5) . ? C2 C3 1.368(5) . ? C2 H2 0.9300 . ? C3 C4 1.395(6) . ? C3 H3 0.9300 . ? C4 C5 1.364(6) . ? C4 H4 0.9300 . ? C5 C6 1.408(5) . ? C5 H5 0.9300 . ? C6 C7 1.519(6) . ? C7 C9 1.528(6) . ? C7 C8 1.533(6) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.379(5) . ? C10 C15 1.409(5) . ? C11 C12 1.382(6) . ? C11 H11 0.9300 . ? C12 C13 1.382(6) . ? C12 H12 0.9300 . ? C13 C14 1.390(6) . ? C13 H13 0.9300 . ? C14 C15 1.398(5) . ? C14 H14 0.9300 . ? C15 C16 1.500(6) . ? C16 C17 1.531(6) . ? C16 C18 1.537(6) . ? C16 H16 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.366(7) . ? C19 H19 0.9300 . ? C20 C21 1.379(7) . ? C20 H20 0.9300 . ? C21 C22 1.361(7) . ? C21 H21 0.9300 . ? C22 C23 1.384(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sn1 O4 90.56(10) . . ? O3 Sn1 O1 76.47(9) . . ? O4 Sn1 O1 75.88(8) . . ? O3 Sn2 O3 91.33(13) 2_655 . ? O3 Sn2 O2 77.16(8) 2_655 2_655 ? O3 Sn2 O2 74.38(8) . 2_655 ? O3 Sn2 O2 74.38(8) 2_655 . ? O3 Sn2 O2 77.16(8) . . ? O2 Sn2 O2 138.83(11) 2_655 . ? O3 Sn3 O4 91.56(10) 2_655 . ? O3 Sn3 O2 75.72(8) 2_655 . ? O4 Sn3 O2 78.51(8) . . ? O3 Sn3 O1 74.65(8) 2_655 2_655 ? O4 Sn3 O1 74.29(8) . 2_655 ? O2 Sn3 O1 138.75(8) . 2_655 ? O4 Sn4 O4 92.29(13) . 2_655 ? O4 Sn4 O1 75.77(8) . 2_655 ? O4 Sn4 O1 75.75(8) 2_655 2_655 ? O4 Sn4 O1 75.75(8) . . ? O4 Sn4 O1 75.77(8) 2_655 . ? O1 Sn4 O1 138.41(11) 2_655 . ? C23 N1 C19 116.3(4) . . ? C1 O1 Sn1 124.5(2) . . ? C1 O1 Sn4 124.6(2) . . ? Sn1 O1 Sn4 93.01(8) . . ? C1 O1 Sn3 121.0(2) . 2_655 ? Sn1 O1 Sn3 92.32(8) . 2_655 ? Sn4 O1 Sn3 92.38(8) . 2_655 ? C10 O2 Sn3 121.42(19) . . ? C10 O2 Sn2 124.7(2) . . ? Sn3 O2 Sn2 94.83(8) . . ? Sn1 O3 Sn3 116.56(11) . 2_655 ? Sn1 O3 Sn2 119.48(11) . . ? Sn3 O3 Sn2 114.92(10) 2_655 . ? Sn4 O4 Sn3 117.42(11) . . ? Sn4 O4 Sn1 115.34(10) . . ? Sn3 O4 Sn1 117.15(11) . . ? O1 C1 C2 119.1(3) . . ? O1 C1 C6 121.7(3) . . ? C2 C1 C6 119.2(3) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 120.1(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 122.5(4) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 117.6(3) . . ? C5 C6 C7 118.4(3) . . ? C1 C6 C7 124.0(3) . . ? C6 C7 C9 111.2(4) . . ? C6 C7 C8 111.6(3) . . ? C9 C7 C8 110.4(3) . . ? C6 C7 H7 107.8 . . ? C9 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 C11 118.8(3) . . ? O2 C10 C15 121.0(3) . . ? C11 C10 C15 120.2(3) . . ? C10 C11 C12 121.2(4) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 118.3(4) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C13 C14 C15 122.8(4) . . ? C13 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C14 C15 C10 117.1(4) . . ? C14 C15 C16 118.4(4) . . ? C10 C15 C16 124.5(3) . . ? C15 C16 C17 112.2(3) . . ? C15 C16 C18 112.9(4) . . ? C17 C16 C18 110.1(3) . . ? C15 C16 H16 107.1 . . ? C17 C16 H16 107.1 . . ? C18 C16 H16 107.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 124.2(5) . . ? N1 C19 H19 117.9 . . ? C20 C19 H19 117.9 . . ? C19 C20 C21 118.0(5) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? C22 C21 C20 119.1(4) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 118.6(4) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? N1 C23 C22 123.8(4) . . ? N1 C23 H23 118.1 . . ? C22 C23 H23 118.1 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.003 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.128 #===END data_11ap221_0m _database_code_depnum_ccdc_archive 'CCDC 843211' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 O8 Sn6, C9 H12 O' _chemical_formula_sum 'C45 H56 O9 Sn6' _chemical_formula_weight 1453.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3902(17) _cell_length_b 13.1348(18) _cell_length_c 16.511(2) _cell_angle_alpha 88.778(2) _cell_angle_beta 72.1440(10) _cell_angle_gamma 75.5470(10) _cell_volume 2472.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 9523 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.20 _exptl_crystal_description Rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 3.034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3560 _exptl_absorpt_correction_T_max 0.6328 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17862 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.23 _reflns_number_total 8846 _reflns_number_gt 6801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+13.4144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8846 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 0.800 _refine_ls_restrained_S_all 0.800 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn6 Sn 0.35494(4) 0.06231(3) 0.21336(3) 0.02804(12) Uani 1 1 d . . . Sn3 Sn 0.08140(4) 0.06202(4) 0.37655(3) 0.03181(13) Uani 1 1 d . . . Sn2 Sn 0.32400(4) -0.16175(3) 0.33422(3) 0.03021(13) Uani 1 1 d . . . Sn5 Sn 0.26735(18) 0.22537(12) 0.40137(12) 0.0246(6) Uani 0.75 1 d P . . Sn1 Sn 0.50208(4) -0.00923(4) 0.37440(3) 0.03150(13) Uani 1 1 d . . . Sn4 Sn 0.22827(4) 0.00525(4) 0.52851(3) 0.03411(13) Uani 1 1 d . . . O1 O 0.3421(3) 0.0863(3) 0.4503(3) 0.0295(9) Uani 1 1 d . . . O2 O 0.2092(3) 0.1426(3) 0.3177(3) 0.0291(9) Uani 1 1 d . . . O3 O 0.4212(4) -0.0477(3) 0.2905(3) 0.0291(9) Uani 1 1 d . . . O4 O 0.4220(4) -0.1362(3) 0.4414(3) 0.0334(10) Uani 1 1 d . . . O5 O 0.1939(3) -0.0498(3) 0.4241(3) 0.0284(9) Uani 1 1 d . . . O6 O 0.2271(4) -0.0560(3) 0.2464(3) 0.0314(9) Uani 1 1 d . . . O7 O 0.0923(3) 0.1519(3) 0.4959(3) 0.0314(9) Uani 1 1 d . . . O8 O 0.4331(3) 0.1672(3) 0.2863(3) 0.0311(9) Uani 1 1 d . . . O9 O 0.1096(5) 0.3070(4) 0.2293(3) 0.0450(12) Uani 1 1 d . . . H9 H 0.1398 0.2553 0.2530 0.067 Uiso 1 1 calc R . . C5 C 0.4740(5) 0.2441(5) 0.2372(4) 0.0330(14) Uani 1 1 d . . . C6 C 0.5969(5) 0.2349(5) 0.2071(4) 0.0328(14) Uani 1 1 d . . . C7 C 0.6830(6) 0.1396(6) 0.2250(4) 0.0390(16) Uani 1 1 d . . . H7 H 0.6464 0.1212 0.2845 0.047 Uiso 1 1 calc R . . C8 C 0.7010(6) 0.0447(6) 0.1664(5) 0.0454(17) Uani 1 1 d . . . H8A H 0.6246 0.0349 0.1680 0.068 Uiso 1 1 calc . . . H8B H 0.7457 -0.0183 0.1856 0.068 Uiso 1 1 calc . . . H8C H 0.7443 0.0566 0.1080 0.068 Uiso 1 1 calc . . . C9 C 0.8007(6) 0.1592(7) 0.2217(5) 0.055(2) Uani 1 1 d . . . H9A H 0.8452 0.1664 0.1625 0.083 Uiso 1 1 calc . . . H9B H 0.8453 0.0998 0.2447 0.083 Uiso 1 1 calc . . . H9C H 0.7872 0.2240 0.2558 0.083 Uiso 1 1 calc . . . C10 C 0.6332(6) 0.3181(6) 0.1610(4) 0.0412(17) Uani 1 1 d . . . H10 H 0.7144 0.3155 0.1422 0.049 Uiso 1 1 calc R . . C11 C 0.5558(7) 0.4034(5) 0.1420(5) 0.0471(19) Uani 1 1 d . . . H11 H 0.5834 0.4581 0.1103 0.057 Uiso 1 1 calc R . . C12 C 0.4377(6) 0.4078(6) 0.1700(5) 0.0450(18) Uani 1 1 d . . . H12 H 0.3835 0.4659 0.1570 0.054 Uiso 1 1 calc R . . C13 C 0.3969(6) 0.3284(5) 0.2170(4) 0.0387(16) Uani 1 1 d . . . H13 H 0.3153 0.3322 0.2353 0.046 Uiso 1 1 calc R . . C16 C 0.1952(5) -0.0952(4) 0.1812(4) 0.0235(12) Uani 1 1 d . . . C17 C 0.2803(5) -0.1597(5) 0.1132(4) 0.0325(14) Uani 1 1 d . . . C18 C 0.4114(6) -0.1930(5) 0.1015(4) 0.0363(15) Uani 1 1 d . . . H18 H 0.4251 -0.1579 0.1493 0.044 Uiso 1 1 calc R . . C19 C 0.4818(7) -0.1554(7) 0.0168(5) 0.055(2) Uani 1 1 d . . . H19A H 0.4723 -0.1908 -0.0313 0.083 Uiso 1 1 calc . . . H19B H 0.5650 -0.1725 0.0127 0.083 Uiso 1 1 calc . . . H19C H 0.4526 -0.0791 0.0153 0.083 Uiso 1 1 calc . . . C20 C 0.4546(7) -0.3123(6) 0.1062(6) 0.053(2) Uani 1 1 d . . . H20A H 0.4081 -0.3343 0.1599 0.079 Uiso 1 1 calc . . . H20B H 0.5373 -0.3303 0.1034 0.079 Uiso 1 1 calc . . . H20C H 0.4459 -0.3486 0.0582 0.079 Uiso 1 1 calc . . . C21 C 0.2405(6) -0.1948(6) 0.0512(5) 0.0423(16) Uani 1 1 d . . . H21 H 0.2962 -0.2386 0.0041 0.051 Uiso 1 1 calc R . . C22 C 0.1218(6) -0.1685(6) 0.0551(5) 0.0426(17) Uani 1 1 d . . . H22 H 0.0972 -0.1953 0.0127 0.051 Uiso 1 1 calc R . . C23 C 0.0419(6) -0.1022(5) 0.1227(5) 0.0407(16) Uani 1 1 d . . . H23 H -0.0386 -0.0813 0.1261 0.049 Uiso 1 1 calc R . . C24 C 0.0784(5) -0.0663(5) 0.1849(4) 0.0328(14) Uani 1 1 d . . . H24 H 0.0226 -0.0210 0.2310 0.039 Uiso 1 1 calc R . . C25 C 0.0048(5) 0.2259(4) 0.5559(4) 0.0251(12) Uani 1 1 d . . . C26 C -0.0655(5) 0.3133(5) 0.5300(4) 0.0329(14) Uani 1 1 d . . . C27 C -0.0585(6) 0.3335(5) 0.4380(4) 0.0353(15) Uani 1 1 d . . . H27 H 0.0128 0.2816 0.4014 0.042 Uiso 1 1 calc R . . C28 C -0.0449(7) 0.4434(6) 0.4129(5) 0.0468(18) Uani 1 1 d . . . H28A H -0.1106 0.4966 0.4504 0.070 Uiso 1 1 calc . . . H28B H -0.0444 0.4523 0.3537 0.070 Uiso 1 1 calc . . . H28C H 0.0289 0.4518 0.4185 0.070 Uiso 1 1 calc . . . C29 C -0.1649(7) 0.3129(6) 0.4182(6) 0.053(2) Uani 1 1 d . . . H29A H -0.1716 0.2418 0.4336 0.079 Uiso 1 1 calc . . . H29B H -0.1546 0.3193 0.3572 0.079 Uiso 1 1 calc . . . H29C H -0.2363 0.3646 0.4512 0.079 Uiso 1 1 calc . . . C30 C -0.1487(6) 0.3853(6) 0.5946(4) 0.0402(16) Uani 1 1 d . . . H30 H -0.1981 0.4448 0.5790 0.048 Uiso 1 1 calc R . . C31 C -0.1612(6) 0.3726(6) 0.6804(5) 0.0454(18) Uani 1 1 d . . . H31 H -0.2186 0.4227 0.7223 0.055 Uiso 1 1 calc R . . C32 C -0.0901(6) 0.2868(6) 0.7048(5) 0.0425(17) Uani 1 1 d . . . H32 H -0.0972 0.2779 0.7632 0.051 Uiso 1 1 calc R . . C33 C -0.0078(6) 0.2135(6) 0.6418(4) 0.0371(15) Uani 1 1 d . . . H33 H 0.0408 0.1539 0.6581 0.045 Uiso 1 1 calc R . . C34 C 0.4752(5) -0.2281(5) 0.4731(4) 0.0295(13) Uani 1 1 d . . . C35 C 0.5742(6) -0.3018(5) 0.4168(4) 0.0373(15) Uani 1 1 d . . . C36 C 0.6346(6) -0.2853(6) 0.3241(4) 0.0401(16) Uani 1 1 d . . . H36 H 0.5843 -0.2217 0.3073 0.048 Uiso 1 1 calc R . . C37 C 0.7551(6) -0.2625(7) 0.3142(5) 0.056(2) Uani 1 1 d . . . H37A H 0.7451 -0.2071 0.3567 0.083 Uiso 1 1 calc . . . H37B H 0.7864 -0.2393 0.2569 0.083 Uiso 1 1 calc . . . H37C H 0.8099 -0.3268 0.3228 0.083 Uiso 1 1 calc . . . C38 C 0.6490(8) -0.3780(7) 0.2642(5) 0.059(2) Uani 1 1 d . . . H38A H 0.7050 -0.4398 0.2751 0.089 Uiso 1 1 calc . . . H38B H 0.6784 -0.3598 0.2050 0.089 Uiso 1 1 calc . . . H38C H 0.5730 -0.3939 0.2740 0.089 Uiso 1 1 calc . . . C39 C 0.6190(6) -0.3952(6) 0.4524(5) 0.0444(17) Uani 1 1 d . . . H39 H 0.6856 -0.4456 0.4176 0.053 Uiso 1 1 calc R . . C40 C 0.5696(7) -0.4158(6) 0.5362(5) 0.0480(18) Uani 1 1 d . . . H40 H 0.6016 -0.4799 0.5580 0.058 Uiso 1 1 calc R . . C41 C 0.4727(6) -0.3425(5) 0.5884(4) 0.0386(16) Uani 1 1 d . . . H41 H 0.4381 -0.3560 0.6461 0.046 Uiso 1 1 calc R . . C42 C 0.4271(6) -0.2493(5) 0.5555(4) 0.0354(15) Uani 1 1 d . . . H42 H 0.3609 -0.1994 0.5912 0.042 Uiso 1 1 calc R . . C43 C 0.0114(8) 0.5272(7) 0.1447(7) 0.069(3) Uani 1 1 d . . . H43A H -0.0180 0.5441 0.0961 0.103 Uiso 1 1 calc . . . H43B H 0.0055 0.5925 0.1753 0.103 Uiso 1 1 calc . . . H43C H -0.0353 0.4853 0.1832 0.103 Uiso 1 1 calc . . . C44 C 0.1394(7) 0.4642(6) 0.1130(5) 0.0458(17) Uani 1 1 d . . . H44 H 0.1710 0.4594 0.1622 0.055 Uiso 1 1 calc R . . C45 C 0.1470(6) 0.3534(5) 0.0845(4) 0.0376(15) Uani 1 1 d . . . C46 C 0.1282(5) 0.2779(5) 0.1452(4) 0.0353(15) Uani 1 1 d . . . C47 C 0.1289(6) 0.1778(6) 0.1206(5) 0.0460(17) Uani 1 1 d . . . H47 H 0.1149 0.1281 0.1627 0.055 Uiso 1 1 calc R . . C48 C 0.1493(8) 0.1480(7) 0.0361(6) 0.058(2) Uani 1 1 d . . . H48 H 0.1491 0.0788 0.0206 0.070 Uiso 1 1 calc R . . C49 C 0.2109(10) 0.5228(8) 0.0443(6) 0.079(3) Uani 1 1 d . . . H49A H 0.2913 0.4790 0.0207 0.119 Uiso 1 1 calc . . . H49B H 0.2122 0.5891 0.0696 0.119 Uiso 1 1 calc . . . H49C H 0.1750 0.5377 -0.0014 0.119 Uiso 1 1 calc . . . C50 C 0.1676(7) 0.3200(7) -0.0003(5) 0.0492(19) Uani 1 1 d . . . H50 H 0.1807 0.3690 -0.0430 0.059 Uiso 1 1 calc R . . C51 C 0.1699(8) 0.2192(7) -0.0246(5) 0.061(2) Uani 1 1 d . . . H51 H 0.1855 0.1997 -0.0830 0.073 Uiso 1 1 calc R . . Sn5A Sn 0.2665(6) 0.2260(6) 0.4009(5) 0.051(3) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn6 0.0220(2) 0.0305(2) 0.0289(2) 0.00016(17) -0.00414(17) -0.00639(17) Sn3 0.0183(2) 0.0357(3) 0.0424(3) 0.0054(2) -0.00893(18) -0.00952(18) Sn2 0.0237(2) 0.0271(2) 0.0373(2) -0.00117(18) -0.00538(18) -0.00669(17) Sn5 0.0271(13) 0.0174(7) 0.0286(11) -0.0031(7) -0.0068(8) -0.0063(7) Sn1 0.0180(2) 0.0384(3) 0.0380(3) -0.00149(19) -0.00779(18) -0.00779(18) Sn4 0.0322(3) 0.0437(3) 0.0301(2) 0.00341(19) -0.00809(19) -0.0183(2) O1 0.021(2) 0.035(2) 0.031(2) -0.0003(18) -0.0034(17) -0.0093(18) O2 0.022(2) 0.036(2) 0.029(2) -0.0027(18) -0.0065(17) -0.0089(18) O3 0.025(2) 0.032(2) 0.030(2) 0.0014(18) -0.0080(17) -0.0062(18) O4 0.027(2) 0.035(2) 0.036(2) 0.0044(19) -0.0083(19) -0.0048(19) O5 0.020(2) 0.031(2) 0.035(2) -0.0002(18) -0.0070(17) -0.0098(17) O6 0.027(2) 0.032(2) 0.038(2) -0.0014(19) -0.0119(19) -0.0090(18) O7 0.022(2) 0.034(2) 0.033(2) -0.0022(19) -0.0028(18) -0.0032(18) O8 0.023(2) 0.031(2) 0.038(2) 0.0010(19) -0.0059(18) -0.0101(18) O9 0.050(3) 0.039(3) 0.038(3) -0.004(2) -0.008(2) -0.002(2) C5 0.028(3) 0.033(3) 0.033(3) -0.006(3) 0.002(3) -0.011(3) C6 0.024(3) 0.039(4) 0.034(3) -0.008(3) -0.005(3) -0.010(3) C7 0.024(3) 0.051(4) 0.041(4) 0.005(3) -0.005(3) -0.015(3) C8 0.034(4) 0.047(4) 0.049(4) -0.002(3) -0.005(3) -0.009(3) C9 0.027(4) 0.076(6) 0.064(5) 0.004(4) -0.010(4) -0.020(4) C10 0.026(3) 0.046(4) 0.044(4) -0.003(3) 0.006(3) -0.016(3) C11 0.049(4) 0.030(4) 0.053(4) 0.004(3) 0.005(3) -0.020(3) C12 0.038(4) 0.035(4) 0.049(4) 0.003(3) 0.001(3) -0.005(3) C13 0.027(3) 0.038(4) 0.042(4) 0.001(3) -0.001(3) -0.005(3) C16 0.026(3) 0.018(3) 0.025(3) 0.000(2) -0.007(2) -0.005(2) C17 0.028(3) 0.031(3) 0.041(4) 0.006(3) -0.012(3) -0.010(3) C18 0.028(3) 0.034(4) 0.045(4) -0.001(3) -0.008(3) -0.008(3) C19 0.035(4) 0.077(6) 0.046(4) 0.001(4) 0.002(3) -0.019(4) C20 0.050(5) 0.042(4) 0.067(5) -0.004(4) -0.027(4) -0.001(4) C21 0.040(4) 0.046(4) 0.041(4) 0.000(3) -0.013(3) -0.013(3) C22 0.041(4) 0.043(4) 0.048(4) -0.008(3) -0.018(3) -0.012(3) C23 0.029(3) 0.040(4) 0.057(4) -0.001(3) -0.019(3) -0.010(3) C24 0.023(3) 0.032(3) 0.037(3) -0.007(3) -0.002(3) -0.004(3) C25 0.020(3) 0.021(3) 0.035(3) -0.006(2) -0.007(2) -0.008(2) C26 0.018(3) 0.034(4) 0.043(4) -0.003(3) -0.002(3) -0.008(3) C27 0.029(3) 0.039(4) 0.037(4) -0.003(3) -0.011(3) -0.007(3) C28 0.049(4) 0.043(4) 0.051(4) 0.006(3) -0.019(4) -0.013(3) C29 0.037(4) 0.047(5) 0.075(6) -0.005(4) -0.026(4) -0.002(3) C30 0.031(4) 0.040(4) 0.048(4) 0.004(3) -0.005(3) -0.014(3) C31 0.039(4) 0.040(4) 0.042(4) -0.013(3) 0.013(3) -0.013(3) C32 0.042(4) 0.042(4) 0.045(4) -0.003(3) -0.003(3) -0.025(3) C33 0.033(4) 0.042(4) 0.037(4) -0.002(3) -0.009(3) -0.012(3) C34 0.021(3) 0.022(3) 0.050(4) 0.001(3) -0.016(3) -0.007(2) C35 0.027(3) 0.043(4) 0.043(4) 0.000(3) -0.010(3) -0.011(3) C36 0.028(3) 0.041(4) 0.044(4) 0.003(3) -0.006(3) -0.003(3) C37 0.025(4) 0.071(6) 0.053(5) 0.011(4) 0.006(3) -0.005(4) C38 0.055(5) 0.061(5) 0.047(5) -0.007(4) -0.007(4) -0.001(4) C39 0.034(4) 0.041(4) 0.051(4) 0.002(3) -0.010(3) -0.001(3) C40 0.044(4) 0.043(4) 0.060(5) 0.014(4) -0.024(4) -0.007(3) C41 0.046(4) 0.041(4) 0.040(4) 0.008(3) -0.020(3) -0.022(3) C42 0.030(3) 0.039(4) 0.038(4) -0.001(3) -0.008(3) -0.013(3) C43 0.053(5) 0.056(6) 0.090(7) -0.012(5) -0.026(5) 0.008(4) C44 0.049(4) 0.041(4) 0.047(4) 0.004(3) -0.015(3) -0.011(3) C45 0.028(3) 0.041(4) 0.042(4) 0.009(3) -0.011(3) -0.005(3) C46 0.023(3) 0.042(4) 0.038(4) 0.000(3) -0.010(3) -0.003(3) C47 0.038(4) 0.039(4) 0.064(5) 0.002(4) -0.019(4) -0.011(3) C48 0.066(6) 0.054(5) 0.061(5) -0.012(4) -0.032(5) -0.011(4) C49 0.103(8) 0.054(6) 0.075(6) 0.010(5) -0.007(6) -0.036(6) C50 0.048(4) 0.062(5) 0.035(4) 0.010(4) -0.010(3) -0.013(4) C51 0.066(6) 0.064(6) 0.047(5) -0.015(4) -0.017(4) -0.008(5) Sn5A 0.014(4) 0.076(5) 0.061(5) 0.000(4) -0.009(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn6 O3 2.086(4) . ? Sn6 O2 2.135(4) . ? Sn6 O8 2.396(4) . ? Sn6 O6 2.425(4) . ? Sn3 O5 2.077(4) . ? Sn3 O2 2.103(4) . ? Sn3 O7 2.374(4) . ? Sn2 O5 2.099(4) . ? Sn2 O3 2.130(4) . ? Sn2 O6 2.372(4) . ? Sn2 O4 2.504(4) . ? Sn5 O1 2.098(5) . ? Sn5 O2 2.163(4) . ? Sn5 O8 2.301(5) . ? Sn1 O3 2.077(4) . ? Sn1 O1 2.091(4) . ? Sn1 O4 2.250(4) . ? Sn4 O5 2.082(4) . ? Sn4 O1 2.089(4) . ? Sn4 O7 2.393(4) . ? O1 Sn5A 2.112(9) . ? O2 Sn5A 2.155(9) . ? O4 C34 1.397(7) . ? O6 C16 1.402(7) . ? O7 C25 1.399(7) . ? O8 C5 1.381(7) . ? O8 Sn5A 2.304(8) . ? O9 C46 1.382(8) . ? O9 H9 0.8400 . ? C5 C13 1.379(9) . ? C5 C6 1.423(9) . ? C6 C10 1.405(9) . ? C6 C7 1.518(9) . ? C7 C8 1.523(10) . ? C7 C9 1.528(9) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.382(10) . ? C10 H10 0.9500 . ? C11 C12 1.380(10) . ? C11 H11 0.9500 . ? C12 C13 1.391(9) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C16 C24 1.384(8) . ? C16 C17 1.400(9) . ? C17 C21 1.395(9) . ? C17 C18 1.524(9) . ? C18 C20 1.532(10) . ? C18 C19 1.550(10) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.405(10) . ? C21 H21 0.9500 . ? C22 C23 1.384(10) . ? C22 H22 0.9500 . ? C23 C24 1.375(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C33 1.390(9) . ? C25 C26 1.403(9) . ? C26 C30 1.406(9) . ? C26 C27 1.516(9) . ? C27 C28 1.529(10) . ? C27 C29 1.537(10) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.388(10) . ? C30 H30 0.9500 . ? C31 C32 1.381(11) . ? C31 H31 0.9500 . ? C32 C33 1.397(10) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C42 1.361(9) . ? C34 C35 1.433(9) . ? C35 C39 1.410(10) . ? C35 C36 1.521(9) . ? C36 C38 1.526(11) . ? C36 C37 1.554(10) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.382(10) . ? C39 H39 0.9500 . ? C40 C41 1.391(10) . ? C40 H40 0.9500 . ? C41 C42 1.388(9) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.525(11) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.510(10) . ? C44 C49 1.534(11) . ? C44 H44 1.0000 . ? C45 C50 1.402(10) . ? C45 C46 1.405(9) . ? C46 C47 1.381(10) . ? C47 C48 1.386(11) . ? C47 H47 0.9500 . ? C48 C51 1.367(12) . ? C48 H48 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.383(12) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sn6 O2 93.11(16) . . ? O3 Sn6 O8 78.99(15) . . ? O2 Sn6 O8 74.87(14) . . ? O3 Sn6 O6 74.51(15) . . ? O2 Sn6 O6 75.91(15) . . ? O8 Sn6 O6 138.99(14) . . ? O5 Sn3 O2 94.07(16) . . ? O5 Sn3 O7 75.98(15) . . ? O2 Sn3 O7 78.60(15) . . ? O5 Sn2 O3 90.53(16) . . ? O5 Sn2 O6 78.45(15) . . ? O3 Sn2 O6 74.90(15) . . ? O5 Sn2 O4 76.63(15) . . ? O3 Sn2 O4 71.66(14) . . ? O6 Sn2 O4 137.64(14) . . ? O1 Sn5 O2 93.25(17) . . ? O1 Sn5 O8 81.87(16) . . ? O2 Sn5 O8 76.38(16) . . ? O3 Sn1 O1 90.54(16) . . ? O3 Sn1 O4 78.10(16) . . ? O1 Sn1 O4 81.37(16) . . ? O5 Sn4 O1 91.43(16) . . ? O5 Sn4 O7 75.46(15) . . ? O1 Sn4 O7 78.84(15) . . ? Sn4 O1 Sn1 115.0(2) . . ? Sn4 O1 Sn5 117.53(19) . . ? Sn1 O1 Sn5 118.38(19) . . ? Sn4 O1 Sn5A 117.4(3) . . ? Sn1 O1 Sn5A 118.4(3) . . ? Sn5 O1 Sn5A 0.2(3) . . ? Sn3 O2 Sn6 117.68(19) . . ? Sn3 O2 Sn5A 116.6(3) . . ? Sn6 O2 Sn5A 110.6(3) . . ? Sn3 O2 Sn5 116.54(19) . . ? Sn6 O2 Sn5 110.43(18) . . ? Sn5A O2 Sn5 0.4(3) . . ? Sn1 O3 Sn6 122.2(2) . . ? Sn1 O3 Sn2 114.21(18) . . ? Sn6 O3 Sn2 114.92(18) . . ? C34 O4 Sn1 129.1(4) . . ? C34 O4 Sn2 115.8(4) . . ? Sn1 O4 Sn2 95.87(15) . . ? Sn3 O5 Sn4 114.26(19) . . ? Sn3 O5 Sn2 116.07(19) . . ? Sn4 O5 Sn2 120.49(19) . . ? C16 O6 Sn2 124.7(3) . . ? C16 O6 Sn6 119.7(3) . . ? Sn2 O6 Sn6 95.63(14) . . ? C25 O7 Sn3 129.6(3) . . ? C25 O7 Sn4 125.3(4) . . ? Sn3 O7 Sn4 94.24(15) . . ? C5 O8 Sn5 116.1(4) . . ? C5 O8 Sn5A 115.9(4) . . ? Sn5 O8 Sn5A 0.4(3) . . ? C5 O8 Sn6 112.6(4) . . ? Sn5 O8 Sn6 97.41(15) . . ? Sn5A O8 Sn6 97.2(2) . . ? C46 O9 H9 109.5 . . ? C13 C5 O8 120.4(6) . . ? C13 C5 C6 120.5(6) . . ? O8 C5 C6 119.1(6) . . ? C10 C6 C5 116.7(6) . . ? C10 C6 C7 122.4(6) . . ? C5 C6 C7 120.9(6) . . ? C6 C7 C8 111.1(6) . . ? C6 C7 C9 114.2(6) . . ? C8 C7 C9 110.7(6) . . ? C6 C7 H7 106.8 . . ? C8 C7 H7 106.8 . . ? C9 C7 H7 106.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C6 122.8(6) . . ? C11 C10 H10 118.6 . . ? C6 C10 H10 118.6 . . ? C12 C11 C10 118.7(6) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 120.8(7) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C5 C13 C12 120.4(6) . . ? C5 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C24 C16 C17 121.2(6) . . ? C24 C16 O6 118.3(5) . . ? C17 C16 O6 120.5(5) . . ? C21 C17 C16 116.5(6) . . ? C21 C17 C18 118.2(6) . . ? C16 C17 C18 125.3(6) . . ? C17 C18 C20 111.6(6) . . ? C17 C18 C19 110.8(6) . . ? C20 C18 C19 111.0(6) . . ? C17 C18 H18 107.8 . . ? C20 C18 H18 107.8 . . ? C19 C18 H18 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 C22 123.0(7) . . ? C17 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C23 C22 C21 117.9(6) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C24 C23 C22 120.4(6) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C16 120.9(6) . . ? C23 C24 H24 119.5 . . ? C16 C24 H24 119.5 . . ? C33 C25 O7 118.5(5) . . ? C33 C25 C26 120.5(6) . . ? O7 C25 C26 120.9(5) . . ? C25 C26 C30 116.9(6) . . ? C25 C26 C27 124.4(6) . . ? C30 C26 C27 118.7(6) . . ? C26 C27 C28 113.7(6) . . ? C26 C27 C29 110.8(6) . . ? C28 C27 C29 110.4(6) . . ? C26 C27 H27 107.2 . . ? C28 C27 H27 107.2 . . ? C29 C27 H27 107.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C26 122.4(7) . . ? C31 C30 H30 118.8 . . ? C26 C30 H30 118.8 . . ? C32 C31 C30 119.9(6) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 118.8(7) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C25 C33 C32 121.5(7) . . ? C25 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C42 C34 O4 119.3(6) . . ? C42 C34 C35 121.1(6) . . ? O4 C34 C35 119.4(6) . . ? C39 C35 C34 116.1(6) . . ? C39 C35 C36 118.8(6) . . ? C34 C35 C36 125.1(6) . . ? C35 C36 C38 112.6(6) . . ? C35 C36 C37 110.3(6) . . ? C38 C36 C37 110.8(6) . . ? C35 C36 H36 107.7 . . ? C38 C36 H36 107.7 . . ? C37 C36 H36 107.7 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C35 122.3(7) . . ? C40 C39 H39 118.8 . . ? C35 C39 H39 118.8 . . ? C39 C40 C41 119.7(7) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 119.4(6) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C34 C42 C41 121.4(6) . . ? C34 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C43 110.0(7) . . ? C45 C44 C49 113.9(7) . . ? C43 C44 C49 110.1(7) . . ? C45 C44 H44 107.5 . . ? C43 C44 H44 107.5 . . ? C49 C44 H44 107.5 . . ? C50 C45 C46 116.1(7) . . ? C50 C45 C44 124.1(6) . . ? C46 C45 C44 119.7(6) . . ? C47 C46 O9 121.7(6) . . ? C47 C46 C45 120.4(7) . . ? O9 C46 C45 118.0(6) . . ? C46 C47 C48 121.8(8) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C51 C48 C47 119.2(8) . . ? C51 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 C45 123.2(7) . . ? C51 C50 H50 118.4 . . ? C45 C50 H50 118.4 . . ? C48 C51 C50 119.3(8) . . ? C48 C51 H51 120.3 . . ? C50 C51 H51 120.3 . . ? O1 Sn5A O2 93.1(3) . . ? O1 Sn5A O8 81.5(3) . . ? O2 Sn5A O8 76.5(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.23 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.352 _refine_diff_density_min -1.373 _refine_diff_density_rms 0.155 #===END data_10fb091new _database_code_depnum_ccdc_archive 'CCDC 843212' #TrackingRef '- Boyle. DT-ART-01- 2012-030108 Updated_CIF_SnOR.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H60 O7 Sn4' _chemical_formula_sum 'C39 H60 O7 Sn4' _chemical_formula_weight 1115.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall -P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 22.7442(13) _cell_length_b 16.4148(9) _cell_length_c 23.7362(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8861.7(9) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9750 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.22 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4400 _exptl_absorpt_coefficient_mu 2.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6595 _exptl_absorpt_correction_T_max 0.7723 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 61596 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8018 _reflns_number_gt 6596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1547P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8018 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.810 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.031170(12) 1.042705(17) 0.270798(13) 0.03029(10) Uani 1 1 d . . . Sn2 Sn 0.155094(13) 0.910057(18) 0.276012(12) 0.03317(10) Uani 1 1 d . . . Sn3 Sn 0.049867(13) 0.910203(17) 0.387377(12) 0.03157(10) Uani 1 1 d . . . Sn4 Sn 0.004463(14) 0.811691(19) 0.245290(15) 0.04163(11) Uani 1 1 d . . . O1 O 0.12116(13) 1.02452(17) 0.22788(12) 0.0337(7) Uani 1 1 d . . . O2 O 0.13876(11) 0.84943(15) 0.36420(11) 0.0276(6) Uani 1 1 d . . . O3 O -0.00953(12) 1.01591(18) 0.35613(12) 0.0356(7) Uani 1 1 d . . . O4 O 0.00071(12) 0.82486(17) 0.33364(15) 0.0408(7) Uani 1 1 d . . . O5 O -0.00984(14) 0.93718(18) 0.22966(14) 0.0389(7) Uani 1 1 d . . . O6 O 0.09599(14) 0.82304(18) 0.23505(13) 0.0395(7) Uani 1 1 d . . . O7 O 0.07823(12) 0.95195(17) 0.31018(12) 0.0344(7) Uani 1 1 d . . . C1 C 0.14764(18) 1.0769(2) 0.19140(18) 0.0318(9) Uani 1 1 d . . . C2 C 0.17481(19) 1.1481(3) 0.21167(19) 0.0376(10) Uani 1 1 d . . . C3 C 0.2020(2) 1.1993(3) 0.1728(2) 0.0514(13) Uani 1 1 d . . . H3 H 0.2206 1.2463 0.1857 0.062 Uiso 1 1 calc R . . C4 C 0.2022(3) 1.1826(4) 0.1161(2) 0.0664(18) Uani 1 1 d . . . H4 H 0.2208 1.2178 0.0910 0.080 Uiso 1 1 calc R . . C5 C 0.1748(3) 1.1136(5) 0.0966(2) 0.0675(17) Uani 1 1 d . . . H5 H 0.1746 1.1026 0.0582 0.081 Uiso 1 1 calc R . . C6 C 0.1472(2) 1.0596(4) 0.1335(2) 0.0502(12) Uani 1 1 d . . . C7 C 0.1180(3) 0.9825(4) 0.1122(2) 0.0708(19) Uani 1 1 d . . . H7 H 0.0977 0.9568 0.1440 0.085 Uiso 1 1 calc R . . C8 C 0.1610(4) 0.9224(6) 0.0892(5) 0.118(2) Uani 1 1 d . . . H8A H 0.1833 0.9473 0.0594 0.177 Uiso 1 1 calc . . . H8B H 0.1403 0.8760 0.0747 0.177 Uiso 1 1 calc . . . H8C H 0.1872 0.9054 0.1186 0.177 Uiso 1 1 calc . . . C9 C 0.0723(4) 1.0011(6) 0.0673(4) 0.118(2) Uani 1 1 d . . . H9A H 0.0912 1.0250 0.0351 0.177 Uiso 1 1 calc . . . H9B H 0.0438 1.0386 0.0821 0.177 Uiso 1 1 calc . . . H9C H 0.0530 0.9516 0.0563 0.177 Uiso 1 1 calc . . . C10 C 0.1749(2) 1.1674(3) 0.2742(2) 0.0470(12) Uani 1 1 d . . . H10 H 0.1396 1.1433 0.2909 0.056 Uiso 1 1 calc R . . C11 C 0.1743(3) 1.2597(4) 0.2868(3) 0.0752(13) Uani 1 1 d . . . H11A H 0.2103 1.2838 0.2737 0.113 Uiso 1 1 calc . . . H11B H 0.1706 1.2682 0.3266 0.113 Uiso 1 1 calc . . . H11C H 0.1416 1.2846 0.2678 0.113 Uiso 1 1 calc . . . C12 C 0.2285(3) 1.1296(4) 0.3030(3) 0.0752(13) Uani 1 1 d . . . H12A H 0.2296 1.0722 0.2951 0.113 Uiso 1 1 calc . . . H12B H 0.2258 1.1379 0.3429 0.113 Uiso 1 1 calc . . . H12C H 0.2636 1.1548 0.2889 0.113 Uiso 1 1 calc . . . C13 C 0.17557(17) 0.8074(2) 0.39868(16) 0.0262(8) Uani 1 1 d . . . C14 C 0.15974(17) 0.7279(2) 0.41589(16) 0.0266(8) Uani 1 1 d . . . C15 C 0.19780(19) 0.6851(2) 0.45101(17) 0.0332(9) Uani 1 1 d . . . H15 H 0.1875 0.6329 0.4628 0.040 Uiso 1 1 calc R . . C16 C 0.25063(18) 0.7184(3) 0.46885(18) 0.0367(10) Uani 1 1 d . . . H16 H 0.2763 0.6883 0.4911 0.044 Uiso 1 1 calc R . . C17 C 0.26436(18) 0.7968(3) 0.45296(18) 0.0346(10) Uani 1 1 d . . . H17 H 0.2994 0.8196 0.4657 0.041 Uiso 1 1 calc R . . C18 C 0.22796(17) 0.8431(2) 0.41872(16) 0.0275(8) Uani 1 1 d . . . C19 C 0.2409(2) 0.9319(3) 0.4067(2) 0.0388(10) Uani 1 1 d . . . H19 H 0.2195 0.9468 0.3724 0.047 Uiso 1 1 calc R . . C20 C 0.2174(3) 0.9838(3) 0.4539(3) 0.0687(18) Uani 1 1 d . . . H20A H 0.1767 0.9713 0.4600 0.103 Uiso 1 1 calc . . . H20B H 0.2214 1.0403 0.4441 0.103 Uiso 1 1 calc . . . H20C H 0.2392 0.9729 0.4877 0.103 Uiso 1 1 calc . . . C21 C 0.3049(3) 0.9505(4) 0.3969(3) 0.073(2) Uani 1 1 d . . . H21A H 0.3261 0.9456 0.4317 0.110 Uiso 1 1 calc . . . H21B H 0.3089 1.0051 0.3827 0.110 Uiso 1 1 calc . . . H21C H 0.3207 0.9128 0.3699 0.110 Uiso 1 1 calc . . . C22 C 0.10134(18) 0.6933(2) 0.39632(18) 0.0342(10) Uani 1 1 d . . . H22 H 0.0729 0.7382 0.3966 0.041 Uiso 1 1 calc R . . C23 C 0.1056(2) 0.6629(3) 0.3358(2) 0.0445(11) Uani 1 1 d . . . H23A H 0.1211 0.7053 0.3122 0.067 Uiso 1 1 calc . . . H23B H 0.0672 0.6477 0.3226 0.067 Uiso 1 1 calc . . . H23C H 0.1311 0.6164 0.3343 0.067 Uiso 1 1 calc . . . C24 C 0.0767(2) 0.6267(3) 0.4347(2) 0.0510(13) Uani 1 1 d . . . H24A H 0.0383 0.6111 0.4218 0.076 Uiso 1 1 calc . . . H24B H 0.0741 0.6469 0.4726 0.076 Uiso 1 1 calc . . . H24C H 0.1023 0.5802 0.4338 0.076 Uiso 1 1 calc . . . C25 C -0.04549(18) 1.0669(3) 0.38559(17) 0.0307(9) Uani 1 1 d . . . C26 C -0.10680(18) 1.0554(3) 0.38301(18) 0.0326(9) Uani 1 1 d . . . C27 C -0.1432(2) 1.1072(3) 0.4137(2) 0.0413(11) Uani 1 1 d . . . H27 H -0.1837 1.1002 0.4121 0.050 Uiso 1 1 calc R . . C28 C -0.1201(2) 1.1685(3) 0.4464(2) 0.0472(12) Uani 1 1 d . . . H28 H -0.1451 1.2027 0.4666 0.057 Uiso 1 1 calc R . . C29 C -0.0599(2) 1.1793(3) 0.4494(2) 0.0471(12) Uani 1 1 d . . . H29 H -0.0447 1.2203 0.4722 0.057 Uiso 1 1 calc R . . C30 C -0.02166(19) 1.1294(3) 0.41870(18) 0.0376(10) Uani 1 1 d . . . C31 C 0.0445(2) 1.1418(4) 0.4236(2) 0.0521(14) Uani 1 1 d . . . H31 H 0.0630 1.1098 0.3936 0.063 Uiso 1 1 calc R . . C32 C 0.0684(3) 1.1109(4) 0.4788(3) 0.0675(16) Uani 1 1 d . . . H32A H 0.0518 1.1419 0.5092 0.101 Uiso 1 1 calc . . . H32B H 0.1104 1.1168 0.4791 0.101 Uiso 1 1 calc . . . H32C H 0.0583 1.0545 0.4832 0.101 Uiso 1 1 calc . . . C33 C 0.0623(3) 1.2298(5) 0.4150(3) 0.0925(17) Uani 1 1 d . . . H33A H 0.0472 1.2624 0.4453 0.139 Uiso 1 1 calc . . . H33B H 0.0466 1.2492 0.3799 0.139 Uiso 1 1 calc . . . H33C H 0.1044 1.2338 0.4142 0.139 Uiso 1 1 calc . . . C34 C -0.13325(19) 0.9872(3) 0.3478(2) 0.0403(10) Uani 1 1 d . . . H34 H -0.1008 0.9554 0.3318 0.048 Uiso 1 1 calc R . . C35 C -0.1697(3) 1.0210(5) 0.2990(3) 0.0925(17) Uani 1 1 d . . . H35A H -0.1839 0.9768 0.2763 0.139 Uiso 1 1 calc . . . H35B H -0.1457 1.0563 0.2765 0.139 Uiso 1 1 calc . . . H35C H -0.2025 1.0511 0.3137 0.139 Uiso 1 1 calc . . . C36 C -0.1698(4) 0.9308(4) 0.3835(3) 0.090(2) Uani 1 1 d . . . H36A H -0.2039 0.9594 0.3970 0.135 Uiso 1 1 calc . . . H36B H -0.1470 0.9123 0.4150 0.135 Uiso 1 1 calc . . . H36C H -0.1820 0.8849 0.3614 0.135 Uiso 1 1 calc . . . C37 C -0.0435(2) 0.7740(3) 0.3606(3) 0.0565(14) Uani 1 1 d . . . H37A H -0.0741 0.8078 0.3757 0.085 Uiso 1 1 calc . . . H37B H -0.0256 0.7434 0.3905 0.085 Uiso 1 1 calc . . . H37C H -0.0599 0.7372 0.3334 0.085 Uiso 1 1 calc . . . C38 C -0.0512(3) 0.9516(3) 0.1857(3) 0.0702(19) Uani 1 1 d . . . H38A H -0.0609 0.9010 0.1677 0.105 Uiso 1 1 calc . . . H38B H -0.0344 0.9881 0.1585 0.105 Uiso 1 1 calc . . . H38C H -0.0862 0.9754 0.2013 0.105 Uiso 1 1 calc . . . C39 C 0.1215(3) 0.7639(3) 0.1968(2) 0.0593(15) Uani 1 1 d . . . H39A H 0.0929 0.7226 0.1883 0.089 Uiso 1 1 calc . . . H39B H 0.1552 0.7392 0.2142 0.089 Uiso 1 1 calc . . . H39C H 0.1332 0.7906 0.1627 0.089 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02919(17) 0.02449(16) 0.03719(18) 0.00174(12) -0.00334(12) 0.00472(11) Sn2 0.02586(17) 0.04084(19) 0.03280(18) -0.00586(12) 0.00158(11) 0.00855(12) Sn3 0.03274(18) 0.03133(17) 0.03064(17) 0.00262(12) 0.00412(11) 0.00057(12) Sn4 0.0447(2) 0.02853(19) 0.0517(2) -0.00295(13) -0.01652(15) 0.00102(13) O1 0.0282(15) 0.0346(16) 0.0383(17) 0.0023(13) 0.0063(12) 0.0018(12) O2 0.0225(13) 0.0281(14) 0.0321(14) 0.0024(12) -0.0044(11) 0.0033(11) O3 0.0293(15) 0.0448(17) 0.0325(16) 0.0004(14) 0.0039(12) 0.0130(13) O4 0.0351(16) 0.0343(16) 0.053(2) 0.0053(14) -0.0060(14) -0.0042(13) O5 0.0387(17) 0.0320(17) 0.0459(19) -0.0003(14) -0.0161(14) 0.0015(14) O6 0.0446(18) 0.0356(17) 0.0383(17) -0.0111(13) -0.0060(14) 0.0085(15) O7 0.0317(15) 0.0366(16) 0.0349(16) 0.0084(13) 0.0114(13) 0.0137(12) C1 0.029(2) 0.034(2) 0.033(2) 0.0056(18) 0.0061(17) 0.0064(17) C2 0.031(2) 0.039(2) 0.044(2) 0.004(2) 0.0062(19) 0.0057(19) C3 0.041(3) 0.040(3) 0.072(4) 0.015(3) 0.011(3) 0.000(2) C4 0.068(4) 0.074(4) 0.057(4) 0.036(3) 0.028(3) 0.027(3) C5 0.063(4) 0.103(5) 0.037(3) 0.013(3) 0.016(3) 0.012(4) C6 0.040(3) 0.076(3) 0.035(3) -0.004(3) 0.004(2) 0.008(3) C7 0.051(3) 0.117(5) 0.045(3) -0.027(3) 0.005(3) -0.023(4) C8 0.084(4) 0.134(5) 0.135(6) -0.056(5) -0.025(4) 0.020(4) C9 0.084(4) 0.134(5) 0.135(6) -0.056(5) -0.025(4) 0.020(4) C10 0.040(3) 0.055(3) 0.046(3) -0.010(2) 0.011(2) -0.014(2) C11 0.087(3) 0.069(3) 0.069(3) -0.019(2) -0.012(2) 0.008(3) C12 0.087(3) 0.069(3) 0.069(3) -0.019(2) -0.012(2) 0.008(3) C13 0.027(2) 0.0264(19) 0.025(2) -0.0021(16) 0.0013(15) 0.0072(16) C14 0.028(2) 0.0229(19) 0.029(2) -0.0028(16) 0.0028(16) 0.0040(16) C15 0.046(3) 0.0231(19) 0.031(2) -0.0007(17) -0.0002(18) 0.0054(18) C16 0.043(3) 0.037(2) 0.030(2) -0.0046(19) -0.0077(18) 0.013(2) C17 0.030(2) 0.040(2) 0.034(2) -0.0098(19) -0.0066(17) 0.0036(18) C18 0.028(2) 0.030(2) 0.0247(19) -0.0051(16) -0.0031(16) 0.0023(16) C19 0.041(3) 0.036(2) 0.040(3) 0.001(2) -0.008(2) -0.014(2) C20 0.073(4) 0.025(2) 0.108(5) -0.013(3) 0.032(4) -0.006(2) C21 0.058(4) 0.051(3) 0.111(6) -0.010(3) 0.034(4) -0.011(3) C22 0.031(2) 0.026(2) 0.046(3) 0.0020(18) -0.0025(18) 0.0012(17) C23 0.048(3) 0.035(2) 0.050(3) 0.000(2) -0.016(2) -0.005(2) C24 0.049(3) 0.033(2) 0.071(4) 0.004(2) 0.005(3) -0.006(2) C25 0.027(2) 0.036(2) 0.029(2) -0.0011(18) 0.0037(16) 0.0076(17) C26 0.026(2) 0.034(2) 0.038(2) 0.0011(18) 0.0025(17) 0.0079(18) C27 0.033(2) 0.050(3) 0.041(3) 0.002(2) 0.011(2) 0.011(2) C28 0.050(3) 0.051(3) 0.041(3) -0.006(2) 0.014(2) 0.017(2) C29 0.056(3) 0.049(3) 0.037(3) -0.010(2) 0.005(2) -0.001(2) C30 0.031(2) 0.052(3) 0.030(2) -0.004(2) 0.0018(17) -0.003(2) C31 0.040(3) 0.077(4) 0.039(3) -0.017(3) 0.005(2) -0.017(3) C32 0.046(3) 0.084(4) 0.072(4) -0.004(3) -0.010(3) 0.007(3) C33 0.098(4) 0.090(4) 0.090(4) 0.016(3) -0.039(3) -0.024(3) C34 0.030(2) 0.042(2) 0.049(3) -0.003(2) -0.0011(19) 0.001(2) C35 0.098(4) 0.090(4) 0.090(4) 0.016(3) -0.039(3) -0.024(3) C36 0.097(6) 0.072(4) 0.102(6) -0.004(4) 0.004(5) -0.038(4) C37 0.035(3) 0.056(3) 0.078(4) 0.010(3) -0.003(2) -0.013(2) C38 0.081(4) 0.041(3) 0.088(5) -0.002(3) -0.051(4) 0.015(3) C39 0.080(4) 0.052(3) 0.047(3) -0.019(3) -0.002(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O7 2.059(3) . ? Sn1 O5 2.196(3) . ? Sn1 O3 2.270(3) . ? Sn1 O1 2.306(3) . ? Sn2 O7 2.046(3) . ? Sn2 O6 2.189(3) . ? Sn2 O1 2.331(3) . ? Sn2 O2 2.347(3) . ? Sn3 O7 2.060(3) . ? Sn3 O4 2.200(3) . ? Sn3 O3 2.321(3) . ? Sn3 O2 2.321(3) . ? Sn4 O6 2.104(3) . ? Sn4 O4 2.110(3) . ? Sn4 O5 2.118(3) . ? O1 C1 1.361(5) . ? O2 C13 1.359(5) . ? O3 C25 1.363(5) . ? O4 C37 1.455(6) . ? O5 C38 1.424(6) . ? O6 C39 1.450(5) . ? C1 C6 1.403(7) . ? C1 C2 1.406(6) . ? C2 C3 1.393(6) . ? C2 C10 1.517(6) . ? C3 C4 1.376(8) . ? C3 H3 0.9300 . ? C4 C5 1.373(9) . ? C4 H4 0.9300 . ? C5 C6 1.395(8) . ? C5 H5 0.9300 . ? C6 C7 1.518(8) . ? C7 C8 1.493(10) . ? C7 C9 1.519(10) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.528(8) . ? C10 C11 1.545(8) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.410(5) . ? C13 C14 1.414(5) . ? C14 C15 1.392(5) . ? C14 C22 1.518(6) . ? C15 C16 1.386(6) . ? C15 H15 0.9300 . ? C16 C17 1.377(6) . ? C16 H16 0.9300 . ? C17 C18 1.387(6) . ? C17 H17 0.9300 . ? C18 C19 1.514(5) . ? C19 C20 1.505(7) . ? C19 C21 1.506(7) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.525(6) . ? C22 C24 1.530(6) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.402(6) . ? C25 C26 1.408(6) . ? C26 C27 1.392(6) . ? C26 C34 1.521(6) . ? C27 C28 1.374(7) . ? C27 H27 0.9300 . ? C28 C29 1.382(7) . ? C28 H28 0.9300 . ? C29 C30 1.401(6) . ? C29 H29 0.9300 . ? C30 C31 1.522(6) . ? C31 C32 1.506(8) . ? C31 C33 1.515(9) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C36 1.506(8) . ? C34 C35 1.529(8) . ? C34 H34 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Sn1 O5 81.48(12) . . ? O7 Sn1 O3 70.53(10) . . ? O5 Sn1 O3 94.06(12) . . ? O7 Sn1 O1 69.24(10) . . ? O5 Sn1 O1 94.50(11) . . ? O3 Sn1 O1 136.98(10) . . ? O7 Sn2 O6 82.57(12) . . ? O7 Sn2 O1 68.92(10) . . ? O6 Sn2 O1 96.02(11) . . ? O7 Sn2 O2 69.75(10) . . ? O6 Sn2 O2 91.28(10) . . ? O1 Sn2 O2 136.60(9) . . ? O7 Sn3 O4 81.67(12) . . ? O7 Sn3 O3 69.47(10) . . ? O4 Sn3 O3 89.72(11) . . ? O7 Sn3 O2 70.08(10) . . ? O4 Sn3 O2 91.81(10) . . ? O3 Sn3 O2 138.83(9) . . ? O6 Sn4 O4 98.38(11) . . ? O6 Sn4 O5 92.61(12) . . ? O4 Sn4 O5 93.91(12) . . ? C1 O1 Sn1 126.3(2) . . ? C1 O1 Sn2 132.4(2) . . ? Sn1 O1 Sn2 100.47(11) . . ? C13 O2 Sn3 127.7(2) . . ? C13 O2 Sn2 130.9(2) . . ? Sn3 O2 Sn2 99.62(9) . . ? C25 O3 Sn1 125.7(3) . . ? C25 O3 Sn3 130.1(3) . . ? Sn1 O3 Sn3 101.11(10) . . ? C37 O4 Sn4 114.0(3) . . ? C37 O4 Sn3 117.5(3) . . ? Sn4 O4 Sn3 128.39(14) . . ? C38 O5 Sn4 113.0(3) . . ? C38 O5 Sn1 118.4(3) . . ? Sn4 O5 Sn1 128.60(14) . . ? C39 O6 Sn4 114.1(3) . . ? C39 O6 Sn2 118.0(3) . . ? Sn4 O6 Sn2 127.87(14) . . ? Sn2 O7 Sn1 120.49(13) . . ? Sn2 O7 Sn3 120.55(13) . . ? Sn1 O7 Sn3 118.80(13) . . ? O1 C1 C6 119.5(4) . . ? O1 C1 C2 120.1(4) . . ? C6 C1 C2 120.4(4) . . ? C3 C2 C1 118.1(4) . . ? C3 C2 C10 121.3(4) . . ? C1 C2 C10 120.6(4) . . ? C4 C3 C2 121.9(5) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C5 C4 C3 119.5(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.2(5) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 118.9(5) . . ? C5 C6 C7 121.2(5) . . ? C1 C6 C7 119.9(5) . . ? C8 C7 C6 112.7(5) . . ? C8 C7 C9 109.0(6) . . ? C6 C7 C9 111.5(6) . . ? C8 C7 H7 107.9 . . ? C6 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C12 110.7(4) . . ? C2 C10 C11 113.2(4) . . ? C12 C10 C11 108.6(4) . . ? C2 C10 H10 108.0 . . ? C12 C10 H10 108.0 . . ? C11 C10 H10 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 C18 120.9(3) . . ? O2 C13 C14 119.0(3) . . ? C18 C13 C14 120.1(4) . . ? C15 C14 C13 118.7(4) . . ? C15 C14 C22 122.6(4) . . ? C13 C14 C22 118.7(3) . . ? C16 C15 C14 121.5(4) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C15 118.8(4) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 122.5(4) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C17 C18 C13 118.3(4) . . ? C17 C18 C19 121.4(4) . . ? C13 C18 C19 120.0(3) . . ? C20 C19 C21 110.1(4) . . ? C20 C19 C18 109.6(4) . . ? C21 C19 C18 114.4(4) . . ? C20 C19 H19 107.5 . . ? C21 C19 H19 107.5 . . ? C18 C19 H19 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 C23 110.9(4) . . ? C14 C22 C24 113.9(4) . . ? C23 C22 C24 110.5(4) . . ? C14 C22 H22 107.1 . . ? C23 C22 H22 107.1 . . ? C24 C22 H22 107.1 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 C30 120.3(4) . . ? O3 C25 C26 119.3(4) . . ? C30 C25 C26 120.3(4) . . ? C27 C26 C25 118.9(4) . . ? C27 C26 C34 120.1(4) . . ? C25 C26 C34 120.9(4) . . ? C28 C27 C26 121.1(4) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.0(4) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 120.9(5) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C29 C30 C25 118.7(4) . . ? C29 C30 C31 119.8(4) . . ? C25 C30 C31 121.5(4) . . ? C32 C31 C33 110.0(5) . . ? C32 C31 C30 112.3(4) . . ? C33 C31 C30 112.4(5) . . ? C32 C31 H31 107.3 . . ? C33 C31 H31 107.3 . . ? C30 C31 H31 107.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 C26 111.2(5) . . ? C36 C34 C35 110.4(5) . . ? C26 C34 C35 111.3(4) . . ? C36 C34 H34 107.9 . . ? C26 C34 H34 107.9 . . ? C35 C34 H34 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O4 C37 H37A 109.5 . . ? O4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O5 C38 H38A 109.5 . . ? O5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O6 C39 H39A 109.5 . . ? O6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.978 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.098 #===END #===END #===END #===END #===END #===END